Downstream synthetic route of 85908-96-9

85908-96-9 N-Boc-2-Piperidone 7577838, apiperidines compound, is more and more widely used in various fields.

85908-96-9, N-Boc-2-Piperidone is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

85908-96-9, Example 27 – Preparation of Intermediate 6 The synthesis of Intermediate 6 followed the procedure of General Procedure 9 following: Intermediate 6 To a cooled solution (-78OC) of diisopropylamine (8.74 g, 86.4 mmol, 1.6 eq) in THF (200 mL) was added n-BuLi (34.5 mL, 86.4 mmol, 1.6 eq), and the mixture stirred for 1 hour at 0OC. The mixture was cooled to -78OC and to it was added tert-butyl 2- oxopiperidine-1-carboxylate (10.0 g, 54.0 mmol, 1.0 eq). The mixture was stirred for 1 hour and methyl chloroformate (6.12 g, 64.8 mmol, 1.2 eq) was added. The reaction mixture was allowed to warm to room temperature overnight, and was monitored by TLC and LC-MS. After completion, the reaction mixture was quenched with ammonium chloride and evaporated under reduced pressure. The residue was extracted with ethyl acetate (2 x 150 mL), and the combined organic phases were washed with water, brine, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography using silica gel (60-120 mesh) eluting with 40% ethyl acetate in n- hexane to yield 1-(tert-butyl)-3-methyl-2-oxopiperidine-1,3-dicarboxylate (Intermediate 6, 9.2 g, yield: 70%) m/z 202.13 [M-56]+; 1H NMR (400 MHz, DMSO) delta 3.70 (s, 1H), 3.62-3.50 (m, 3H), 2.10-1.89 (m, 2H), 1.88-1.72 (m, 2H), 1.42 (s, 9H) ppm.

85908-96-9 N-Boc-2-Piperidone 7577838, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; VERSEON CORPORATION; SHORT, Kevin Michael; ESTIARTE-MARTINEZ, Maria de los Angeles; KITA, David Ben; SHIAU, Timothy Philip; (340 pag.)WO2016/138532; (2016); A1;,
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Some tips on 21168-72-9

21168-72-9, 21168-72-9 2-(4-(Aminomethyl)piperidin-1-yl)ethanol 7330476, apiperidines compound, is more and more widely used in various fields.

21168-72-9, 2-(4-(Aminomethyl)piperidin-1-yl)ethanol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To the solution of compound 2-(4-(aminomethyl)piperidin-1-yl)ethanol (150 mg, 0.95 mmol) and compound 6-chloro-3-(3-(trifluoromethoxy)phenyl)imidazo[1,2-b]pyridazine (200 mg, 0.64 mmol) in 3 mL DMSO was added DIEA (0.3 mL, 1.37 mmol) and 10 mg CsF, the solvent was stirred for 5 h at 120 C., Then the mixture was purified by HPLC to afford the compound 2-(4-(((3-(3-(trifluoromethoxy)phenyl)imidazo[1,2-b]pyridazin-6-yl)amino)methyl)cyclohexyl)ethanol (34 mg, 8.2%) as a brown solid. (0522) 1H-NMR (CDCl3/400 MHz): delta 8.61 (s, 1H), 8.20-8.25 (m, 1H), 7.95-8.05 (m, 2H), 7.66 (t, J=4.4 Hz, 1H), 7.21-7.28 (m, 1H), 3.80-3.90 (m, 2H), 3.62-3.75 (m, 2H), 3.37 (d, J=6.4 Hz, 2H), 3.21 (t, J=5.2 Hz, 2H), 2.91-3.09 (m, 2H), 2.10 (d, J=14.0 Hz, 2H), 1.51-1.69 (m, 2H). MS (ES+, m/z): (M+H)+: 435.5.

21168-72-9, 21168-72-9 2-(4-(Aminomethyl)piperidin-1-yl)ethanol 7330476, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; Tolero Pharmaceuticals, Inc.; Xu, Yong; Brenning, Benjamin Gary; Kultgen, Steven G.; Liu, Xiaohui; Saunders, Michael; Ho, Koc-Kan; (119 pag.)US9416132; (2016); B2;,
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Brief introduction of 35856-62-3

The synthetic route of 35856-62-3 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.35856-62-3,Piperidine-1-sulfonyl chloride,as a common compound, the synthetic route is as follows.,35856-62-3

1-Methyl-4-(4-nitrophenoxy)piperidine (1.4793 g, 6.26 mmol) was dissolved in 60 mL of EtOH, then Pd/C (209 mg) was added and the mixture was stirred under H2 atmosphere at ambient pressure overnight. The catalyst was filtered off to afford 4-[(1-methylpiperidin-4- yl)oxy]aniline (1.2567 g, 97% yield) as a brown solid, which was used in the next step without further purification.

The synthetic route of 35856-62-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMACYCLICS LLC.; ATALLAH, Gordana, Babic; CHEN, Wei; JIA, Zhaozhong, J.; POZZAN, Alfonso; RAVEGLIA, Lucal, Francesco; ZANALETTI, Riccardo; (815 pag.)WO2016/196776; (2016); A2;,
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Some tips on 19365-08-3

19365-08-3, As the paragraph descriping shows that 19365-08-3 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.19365-08-3,3-Hydroxypiperidin-2-one,as a common compound, the synthetic route is as follows.

General procedure: Potassium carbonate or caesium carbonate (1.5-2.5 eq.) was baked in a reaction vessel under reduced pressure. It was cooled to RT and flooded with argon. Palladium acetate (0.1-0.36 eq.), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (Xantphos, 0.18-0.36 eq.) and dioxane (0.04-0.12M) were added, and the suspension was degassed in an argon stream at room temperature for 10 min. Subsequently, the appropriate amide (1.0-1.2 eq.) and the appropriate 7-chloro-4-oxo-1,4-dihydro-1,8-naphthyridine (1.0 eq.) were added. The mixture was stirred at 80-110 C. for 1 h (or until conversion was complete by analytical HPLC or thin-layer chromatography with appropriate eluent mixtures). The mixture was cooled to RT and all volatile components were removed under reduced pressure, or alternatively the reaction mixture was poured into water, the pH was adjusted to pH 1 with 1M aqueous hydrochloric acid, the mixture was extracted with ethyl acetate, the combined organic phases were washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and filtered, and the solvent was removed under reduced pressure. The crude product was then purified either by normal phase chromatography (eluent: cyclohexane/ethyl acetate mixtures or dichloromethane/methanol mixtures) or preparative RP-HPLC (water/acetonitrile gradient). According to GP2, 150 mg (283 mumol) of the compound from Example 80A were reacted with 39.1 mg (340 mumol) of rac-3-hydroxypiperidin-2-one in the presence of 58.7 mg (425 mumol) of potassium carbonate, 13 mg (57 mumol) of palladium(II) acetate and 33 mg (57 mumol) of Xantphos in 2.5 ml of dioxane. The crude product was purified by means of preparative HPLC (column: Chromatorex C18, 10 mum, 125*40 mm, solvent: acetonitrile/0.1% formic acid gradient; (0 to 3 min. 10% acetonitrile to 40 min. 90% acetonitrile and a further 3 min. 90% acetonitrile), and 102 mg (59% of theory, 100% purity) of the title compound were obtained. 1H NMR (400 MHz, DMSO-d6) delta [ppm]=11.34 (br. d, 1H), 8.89 (s, 1H), 8.70 (d, 1H), 8.17-8.09 (m, 1H), 7.94-7.75 (m, 1H), 7.68-7.56 (m, 2H), 7.41-7.27 (m, 3H), 6.51-6.39 (m, 1H), 5.52-5.46 (m, 1H), 4.27-4.17 (m, 1H), 3.71-3.58 (m, 1H), 3.54-3.40 (m, 1H), 2.12-2.01 (m, 1H), 1.86-1.71 (m, 1H), 1.71-1.57 (m, 1H). LC-MS (Method 3): Rt=2.11 min; 609 [M+H]+. 91.2 mg of the title compound (racemic diastereomer mixture) were separated into the enantiomeric diastereomers by chiral HPLC (preparative HPLC: column: Daicel Chiralpak AZ-H 5 mum 250×30 mm; eluent: 50% isohexane, 20% ethanol; temperature: 25 C.; flow rate: 50 ml/min; UV detection: 220 nm). This gave (in the sequence of elution from the column) 17.8 mg of diastereomer 1 (96.5% de) Rt=3.19 min, 14.5 mg (95% de) of diastereomer 2 Rt=4.21 min, 17.4 mg (97% de) of diastereomer 3 Rt=6.11 min, and 14.5 mg (97% de) of diastereomer 4 Rt=10.80 min. [Analytical HPLC: column: Daicel AZ-3 3 mum 50×4.6 mm; eluent: 50% isohexane, 50% ethanol; temperature: 30 C.; flow rate: 1 ml/min; UV detection: 220 nm] Example 248 1-(2,4-Difluorophenyl)-N-[1-(2,6-difluorophenyl)-2,2,2-trifluoroethyl]-7-[3-hydroxy-2-oxopiperidin-1-yl]-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxamide (diastereomer 1) 1H NMR (400 MHz, DMSO-d6) delta [ppm]=11.34 (br. d, 1H), 8.89 (s, 1H), 8.70 (d, 1H), 8.17-8.10 (m, 1H), 7.93-7.76 (m, 1H), 7.68-7.57 (m, 2H), 7.40-7.27 (m, 3H), 6.51-6.39 (m, 1H), 5.52-5.46 (m, 1H), 4.27-4.18 (m, 1H), 3.71-3.59 (m, 1H), 3.54-3.41 (m, 1H), 2.12-2.01 (m, 1H), 1.83-1.73 (m, 2H), 1.71-1.58 (m, 1H). LC-MS (Method 3): Rt=2.12 min; 609 [M+H]+. Example 249 1-(2,4-Difluorophenyl)-N-[1-(2,6-difluorophenyl)-2,2,2-trifluoroethyl]-7-[3-hydroxy-2-oxopiperidin-1-yl]-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxamide (diastereomer 2) 1H NMR (400 MHz, DMSO-d6) delta [ppm]=11.37-11.31 (m, 1H), 8.89 (s, 1H), 8.70 (d, 1H), 8.13 (dd, 1H), 7.94-7.75 (m, 1H), 7.68-7.56 (m, 2H), 7.41-7.26 (m, 3H), 6.51-6.38 (m, 1H), 5.52-5.46 (m, 1H), 4.27-4.16 (m, 1H), 3.72-3.58 (m, 1H), 3.53-3.39 (m, 1H), 2.12-2.01 (m, 1H), 1.83-1.73 (m, 2H), 1.72-1.57 (m, 1H). LC-MS (Method 3): Rt=2.13 min; 609 [M+H]+. Example 250 1-(2,4-Difluorophenyl)-N-[1-(2,6-difluorophenyl)-2,2,2-trifluoroethyl]-7-[3-hydroxy-2-oxopiperidin-1-yl]-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxamide (3rd diastereomer) 1H NMR (400 MHz, DMSO-d6) delta [ppm]=11.37-11.31 (m, 1H), 8.89 (s, 1H), 8.70 (d, 1H), 8.13 (dd, 1H), 7.94-7.75 (m, 1H), 7.68-7.56 (m, 2H), 7.40-7.26 (m, 3H), 6.51-6.39 (m, 1H), 5.52-5.46 (m, 1H), 4.26-4.17 (m, 1H), 3.72-3.59 (m, 1H), 3.52-3.40 (m, 1H), 2.12-2.01 (m, 1H), 1.84-1.73 (m, 2H), 1.72-1.58 (m, 1H). LC-MS (Method 3): Rt=2.12 min; 609 [M+H]+. Example 251 1-(2,4-Difluorophenyl)-N-[1-(2,6-difluorophenyl)-2,2,2-trifluoroethyl]-7-[3-hydroxy-2-oxopiperidin-1-yl]-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxamide (4th diastereomer) 1H NMR (400 MHz, DMSO-d6) delta [ppm]=11.34 (br. d, 1H), 8.89 (s, 1H), 8.70 (d, 1H), 8.17-8.09 (m, 1H), 7.93-7.76 (m, 1H), 7.68-7.57 (m, 2H), 7.40-7.2…

19365-08-3, As the paragraph descriping shows that 19365-08-3 is playing an increasingly important role.

Reference:
Patent; Bayer Pharma Aktiengesellschaft; TELLER, Henrik; STRAUB, Alexander; BRECHMANN, Markus; MUeLLER, Thomas; MEININGHAUS, Mark; NOWAK-REPPEL, Katrin; TINEL, Hanna; MUeNTER, Klaus; FLIEGNER, Daniela; MONDRITZKI, Thomas; BOULTADAKIS ARAPINIS, Melissa; MARQUARDT, Tobias; VAKALOPOULOS, Alexandros; REBSTOCK, Anne-Sophie; WITTWER, Matthias Beat; (342 pag.)US2018/297994; (2018); A1;,
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Analyzing the synthesis route of 10338-57-5

10338-57-5 4-(Piperidin-1-yl)benzaldehyde 291354, apiperidines compound, is more and more widely used in various fields.

10338-57-5, 4-(Piperidin-1-yl)benzaldehyde is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of compound 1114 (0.34628, 111111110) and 4-piperidin-1-yl-benzaldehyde (0.20818,1.11111111)Wall pressure bottle, then add 2mL of DMS0, 10mL of trimethylchlorosilane, 100 C heating overnight, TLC monitoring reaction after the end,The crude product was purified by silica gel column chromatography (eluent: V (ethyl acetate): V (methanol): V (ammonia) = 10: 1: 0.1)To 0.4090 g of a pale yellow solid in 79% yield., 10338-57-5

10338-57-5 4-(Piperidin-1-yl)benzaldehyde 291354, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; Sun Yat-Sen University; HUANG, ZHISHU; TAN, JIAHENG; WANG, YUQING; (41 pag.)CN106220631; (2016); A;,
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Some tips on 10338-57-5

10338-57-5, 10338-57-5 4-(Piperidin-1-yl)benzaldehyde 291354, apiperidines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.10338-57-5,4-(Piperidin-1-yl)benzaldehyde,as a common compound, the synthetic route is as follows.

Route 2: 1.94g of 4-methoxy-2-methylquinoline and 1.89g of 4-(piperidin-1-yl)benzaldehyde were added to a 250ml round bottom flask with a spherical condenser.The mixture was heated in an oil bath on an Ika magnetic stirrer, and 1.88 g of p-toluenesulfonamide was added as a catalyst, and 8 ml of toluene was used as a solvent, and the mixture was heated under reflux for 72 hours.The solvent was sparged and recrystallized from 2 ml of ethanol to give a pale yellow solid.The yield was 94%.

10338-57-5, 10338-57-5 4-(Piperidin-1-yl)benzaldehyde 291354, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; University of Science and Technology of China; Zhang Guoqing; Chen Biao; Xu Cheng; Huang Wenhuan; Huang Linkun; Bi Guoqiang; (29 pag.)CN110066243; (2019); A;,
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Downstream synthetic route of 1187173-43-8

1187173-43-8, 1187173-43-8 2,7-Diazaspiro[4.5]decan-1-one hydrochloride 45074126, apiperidines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1187173-43-8,2,7-Diazaspiro[4.5]decan-1-one hydrochloride,as a common compound, the synthetic route is as follows.

2,7-Diazaspiro[4.5]decan-1 -one hydrogen chloride (2.314 g, 12.14 mmol) was dissolved in dichloromethane (50 ml_), and triethylamine (8 ml_, 57.4 mmol) was added. The reaction mixture was cooled to 0 C and 4- (trifluoromethyl)benzenesulfonyl chloride (3.27 g, 13.35 mmol) was added. After 2 h, the reaction mixture was washed with aqueous 1 M HCI followed by aqueous 1 M NaOH, the organic layer was passed through a hydrophobic frit, and concentrated in vacuo. The resulting residue was purified by silica column chromatography on SP4 (gradient elution: 0 – 20% DCM – MeOH). The early colourless fractions led to 7-{[4- (trifluoromethyl)phenyl]sulfonyl}-2,7-diazaspiro[4.5]decan-1 -one (360 mg, 0.984 mmol, 8% yield) as a white solid. The later orange fractions were combined, and concentrated in vacuo. The resulting residue was recrystallised from methanol to give 3 batches of white crystals: 1 st batch 7-{[4-(trifluoromethyl)phenyl]sulfonyl}-2,7- diazaspiro[4.5]decan-1 -one (1 .506 g, 4.1 1 mmol, 33% yield), 2nd batch 7-{[4- (trifluoromethyl)phenyl]sulfonyl}-2,7-diazaspiro[4.5]decan-1 -one (400 mg, 1 .093 mmol, 9% yield), and 3rd batch 7-{[4-(trifluoromethyl)phenyl]sulfonyl}-2,7- diazaspiro[4.5]decan-1 -one (324 mg, 0.885 mmol, 7% yield). 1 H NMR (250 MHz, DMSO-d6) 5 ppm 1.31 – 1.76 (m, 4 H) 2.00 (qt, J=13.25, 6.60 Hz, 2 H) 2.18 – 2.32 (m, 2 H) 3.20 (t, J=6.86 Hz, 2 H) 3.34 (d, J=1 1 .49 Hz, 1 H) 3.64 (d, J=1 1 .59 Hz, 1 H) 7.77 (s, 1 H) 7.96 (d, J=8.37 Hz, 2 H) 8.04 (d, J=8.44 Hz, 2 H). MS ES+ve m/z 363 (M+H).

1187173-43-8, 1187173-43-8 2,7-Diazaspiro[4.5]decan-1-one hydrochloride 45074126, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; CONVERGENCE PHARMACEUTICALS LIMITED; GLEAVE, Robert James; HACHISU, Shuji; PAGE, Lee William; BESWICK, Paul John; WO2011/141728; (2011); A1;,
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Brief introduction of 4801-58-5

The synthetic route of 4801-58-5 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4801-58-5,Piperidin-1-ol,as a common compound, the synthetic route is as follows.

To a solution of compound 33a (140mg, 0.588 mmol) in DCM (15 mL) and DIPEA (206 ml, 1.18 mmol) was added dropwise at r.t a solution of triphosgene (69.8 mg, 0.235 mmol) in 5 mL of DCM. After 5 min. a solution of 1-hydroxypiperidine (89.2mg, 0.882 mmol) and DIPEA (103 ml, 0.59 mmol) were added. After stirring overnight at r.t. the reaction mixture was diluted with DCM, the organic layer separated, dried over sodium sulphate and evaporated to dryness. Purification by automated flash chromatography with a Biotage Isolera, FLASH 12+ column, using a gradient from PE : EtOAc 2:8 to EtOAc 100% afforded 13 mg of a white gummy solid, which was repurified on a SNAP 12 RP column with a gradient from NH4HCO3 buffer:ACN 6:4 to NH4HCO3 buffer:ACN 1:1.6 mg of the title compound was obtained as a gummy solid. UPLC-MS [M+H]+ = 366.79 (0376) 1H NMR (400 MHz, CDCl3) d ppm 1.28 (s, 1 H), 1.65 (br. s., 1 H), 1.74 – 1.88 (m, 4 H), 2.39 (s, 3 H), 2.70 (br. s., 2 H), 3.46 (br. s., 2 H), 3.97 (t, 2 H), 4.14 (t, 2 H), 4.91 (s, 2 H), 7.20 – 7.36 (m, 2 H), 7.36 – 7.46 (m, 2 H), 4801-58-5

The synthetic route of 4801-58-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RECORDATI INDUSTRIA CHIMICA E FARMACEUTICA S.P.A; GRAZIANI, Davide; RIVA, Carlo; MENEGON, Sergio; TAZZARI, Valerio; (98 pag.)WO2019/145214; (2019); A1;,
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Simple exploration of 4629-80-5

4629-80-5, The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4629-80-5,1,3-Dimethylpiperidin-4-one,as a common compound, the synthetic route is as follows.

The 3-bromo-i-propoxybenzene (200 g, 0.08703 mol) was combined with THF (540 ml) under nitrogen and cooled to about -75 C. n-Butyl lithium (565 ml, 0.8306 mol) was added dropwise while maintaining the mixture at less than -70 C. After 2 hours 1,3-Dimethyl-4-piperidone (106.7 g, 0.8389 mol) was added while maintaining the temperature of the mixture between -80 C. and -70 C. After stirring 2 hours at -70 C., the reaction mixture was then added to 6N HCl (280 ml) while maintaining the temperature at 20-25 C. The pH was adjusted to 1 with 12 N HCl. The aqueous layer containing product was separated and heptane (320 ml) was added along with 50% NaOH (48 ml, pH=13-14) and the resulting mixture allowed to stand overnight. The mixture was heated to 45-50 C. and the upper layer was separated. The remaining aqueous layer was extracted with heptane (320 ml) at 45-50 C. The combined organic fractions were washed with de-ionized water (120 ml) at 45-50 C. The resulting organic layer was vacuum distilled at a pot temperature of about 55 C. at 100 mmHg. Crystallization from heptane and drying provided 151.8 g of 3-(3-i-propoxyphenyl)-1,3-dimethyl-4-hydroxypiperidine. Melting point 75.0- 76.0 C.

4629-80-5, The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eli Lilly and Company; US5250542; (1993); A;,
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Simple exploration of 1187173-43-8

1187173-43-8, The synthetic route of 1187173-43-8 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1187173-43-8,2,7-Diazaspiro[4.5]decan-1-one hydrochloride,as a common compound, the synthetic route is as follows.

7-{[2-Methyl-5-(trifluoromethyl)phenyl]sulfonyl}-2,7- diazaspiro[4.5]decan-1 -one (2,7-Diazaspiro[4.5]decan-1 -one (200 mg, 1.297 mmol) was dissolved in a mixture of triethylamine (0.542 mL, 3.89 mmol) and dichloromethane (10 mL), and 2-bromo-5- (trifluoromethyl)benzenesulfonyl chloride (503 mg, 1 .556 mmol) was added. The reaction mixture was stirred for 16 h and the reaction mixture was concentrated in vacuo. The resulting yellow solid 7-{[2-bromo-5-(trifluoromethyl)phenyl]sulfonyl}-2,7- diazaspiro[4.5]decan-1 -one (829 mg, impure) was used in the next reaction without further purification. MS ES+ve m/z 443 (M+H).7-{[2-Bromo-5-(trifluoromethyl)phenyl]sulfonyl}-2,7-diazaspiro[4.5]decan-1 -one (829 mg, impure) and potassium carbonate (269 mg, 1.946 mmol) was suspended in 1 ,4- dioxane (20 mL). Trimethylboroxine (0.271 mL, 1.946 mmol) and Pd(PPh3)4 (150 mg, 0.130 mmol) were then added and the reaction mixture was heated to 100 C. After 20 h, the reaction was cooled, filtered through a hydrophobic frit, and concentrated in vacuo. The resulting residue was purified by silica column chromatography on SP4 (gradient elution: 0 – 20% MeOH – DCM). The resulting brown residue was further purified on MDAP to give 7-{[2-methyl-5-(trifluoromethyl)phenyl]sulfonyl}-2,7- diazaspiro[4.5]decan-1 -one (152 mg, 0.400 mmol, 31 % yield) as a white solid. 1 H NMR (400 MHz, DMSO-d6) delta ppm 1 .52 (s, 3 H) 1.63 – 1 .76 (m, 1 H) 1 .91 (t, J=6.88 Hz, 2 H) 2.56 – 2.72 (m, 5 H) 3.04 – 3.20 (m, 2 H) 3.34 – 3.37 (m, 1 H) 3.62 (d, J=1 1 .62 Hz, 1 H) 7.69 – 7.76 (m, 2 H) 7.98 (d, J=8.00 Hz, 1 H) 8.01 (s, 1 H). MS ES+ve m/z 377 (M+H).

1187173-43-8, The synthetic route of 1187173-43-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CONVERGENCE PHARMACEUTICALS LIMITED; GLEAVE, Robert James; HACHISU, Shuji; PAGE, Lee William; BESWICK, Paul John; WO2011/141728; (2011); A1;,
Piperidine – Wikipedia
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