Downstream synthetic route of 85908-96-9

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

Tert-butyl 2-oxopiperidine-1-carboxylate (8.22 g, 41.3 mmol) was dissolved in dry tetrahydrofuran (80 mL) and the system was cooled to -78 C. LiHMDS (1.0 M in THF, 103 mL, 103 mmol) was added dropwise under nitrogen atmosphere. After stirring for a further 20 minutes, 3-bromoprop-1-ene (10.7 mL, 124 mmol) was added. The resulting reaction mixture was stirred at this temperature for 15 minutes. The reaction mixture was then cooled to room temperature and quenched by addition of water (15 mL). The reaction mixture was concentrated under reduced pressure. The resulting residue was diluted with water (30 mL) and extracted with ethyl acetate (50 mL x 3). The combined organic layers were washed with brine (50 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (EtOAc / PE (v / v) = 1/50) to give the title compound as a yellow oil (3.95 g, 35%).

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

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jiatuo Sciences Corporation; Xi Ning; Li Minxiong; Hu Haiyang; Wang Tingjin; (91 pag.)CN104672250; (2017); B;,
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Some tips on 4801-58-5

4801-58-5, 4801-58-5 Piperidin-1-ol 20935, apiperidines compound, is more and more widely used in various fields.

4801-58-5, Piperidin-1-ol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 3; 2-(1 -hvdroxypiperidin-2-yl)-5, -dimethylcvclohexane-1 ,3-dione:; A mixture of N-hydroxypiperidine (1 .01 g, 10 mmol), azodicarbonamide (1 .39 g, 12 mmol) and methanol (10 ml) was heated to reflux for 50 minutes. During this period the solid, initially orange in colour, changed into a whitish precipitate. After cooling to ambient temperature, said precipitate was separated by suction and washed twice with methanol (2 x 5 ml). All the methanol fractions were combined and under agitation 5, 5-dimethylcyclohexane-1 ,3-dione (10 mmol) was added. After 10 minutes, the methanol was removed under vacuum (water bath temperature 50QC) to give a crude compound of formula (3). This crude compound was dissolved in a methanol solution (15 ml) containing acetyl chloride (0.86 g, 1 1 mmol). The methanol was removed under vacuum and the residue of formula (3) in hydrochloride form was ground in acetone.Yield: 62%Formula: C13H22CINO3MW: 275.8 g/molAcid dissociation constants: pKai = 3.47, pKa2 = 6.92 m.p.: 174.5-175.5QC1H-NMR (DMSO-c/e): delta 0.98 (6H, s), 1.48 (1H, m), 1.66 (2H, d, J=12.5 Hz), 1.83 (2H, broad s), 1.94-2.07 (1H, m), 2.33 (4H, broad s), 3.23 (1H, broad s), 3.67 (1H, d, J=11.0 Hz), 4.36 (1 H, d, J=11.5 Hz), 10.93 (1 H, broad s), 11.32 (1 H, broad s). 13C-NMR (DMSO-c/e): delta 21.9, 23.6, 27.9, 28.7, 32.0, 46.2 (broad), 59.4, 64.4, 107.4.

4801-58-5, 4801-58-5 Piperidin-1-ol 20935, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; ABIOGEN PHARMA S.p.A.; NAPOLITANO, Elio; BASAGNI, Simone; TRASCIATTI, Silvia; WO2011/76930; (2011); A1;,
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Some tips on 72752-52-4

As the paragraph descriping shows that 72752-52-4 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.72752-52-4,2-Piperidinobenzonitrile,as a common compound, the synthetic route is as follows.

72752-52-4, To a well stirred suspension of magnesium turnings (67.7 g, 2.80 mol) in THF (30 mL), benzyl chloride (l mL) and catalytic amount of iodine was added at 25-30 C. The contents were stirred for 30 min at 35-40 C. Thereafter, a solution of benzyl chloride (306.0 g, 2.40 mol) dissolved in a mixture of THF (150 mL) and toluene (450 mL) was added, mainraining the intemal temperature of reaction mixture in between 35-45 C. Stirred the reaction mixture for another 2h at 35-40 C and cooled to 25-30 C. Thereafter a solution of nitrile 4 (150,0 g, 0.80 mol) dissolved in THF (150 mL) and toluene (450 mL) was added at 25-45 C. The reaction mixture was cooled to 25-30 C and stirred for 16 h at 25-30 C. The above suspension was added over a mixture of aqueous NH4CI (25% wlw, 600 mL) and aqueous ammonia (300 mL) at 5-15 C. The inorganics were removed through filtration and washed with water (250 mL). The organic layer was separated and concentrated under vacuum to obtained 9 (204.4 g).

As the paragraph descriping shows that 72752-52-4 is playing an increasingly important role.

Reference:
Article; Sundaram, Dhanraj T. S. S.; Mitra, Jayati; Rajesh; Islam, Aminul; Prabahar, Koilpillai Joseph; Rao, Battula Venkateswara; Douglas, Sanasi Paul; Synthetic Communications; vol. 45; 18; (2015); p. 2092 – 2098;,
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Simple exploration of 71985-80-3

71985-80-3, The synthetic route of 71985-80-3 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.71985-80-3,1-Methylpiperidine-4-carboxylic acid hydrochloride,as a common compound, the synthetic route is as follows.

Procedure J Example 90: N-{4-[1,3-benzoxazol-2(3H)-ylidene(cyano)methyl]-2-pyrimidinyl}-2- METHYL-4-PIPERIDINECARBOXAMIDE To a suspension of (2-AMINO-4-PYRIMIDINYL) (1, 3-benzoxazol-2 (3H)-YLIDENE) ethanenitrile (100.00 mg; 0.40 mmol), 1-METHYL-PIPERIDINE-4-CARBOXYLIC acid HCl (107.25 MG ; 0.60 mmol) and 2-CHLORO-1-METHYLPYRIDINIUM iodide (203.37 MG ; 0.80 mmol) in THE (4.00 ML) was added DIEA (0.34 ML ; 1.99 mmol) and the resulting suspension was heated up to 150C under microwave conditions during 900s (normal absorption, 9 bar). After ON standing at 4C, the precipitate formed was filtered off and washed thoroughly with THE then water. After drying at 40C for 2 days, the solid was taken up in DCM to which TFA was added Ether in excess was added and the precipitate obtained was filtered off and washed with ether (3x) then dried under vacuum at 40C. The solid was purified by preparative HPLC to afford after lyophilisation the title compound as a yellow fluffy solid (19%). 1H NMR (METHANOL-D4) 5 : 8.15-7. 95 (m, 1H), 7.47-7. 10 (m, 4H), 6. 83-6. 65 (m, 1H), 3.65- 3. 30 (m, 4H), 3. 16-3. 08 (m, 3H), 3.07-2. 90 (M, 1H), 2.42-1. 90 (M, 4H) M (ES): 375.1 ; M+(ES) : 377.1 ; HPLC (max plot) 98. 1% ; Rt : 2. 00min.

71985-80-3, The synthetic route of 71985-80-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; APPLIED RESEARCH SYSTEMS ARS HOLDING N.V.; WO2005/26159; (2005); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Some tips on 85908-96-9

85908-96-9, The synthetic route of 85908-96-9 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.85908-96-9,N-Boc-2-Piperidone,as a common compound, the synthetic route is as follows.

To a stirred solution of tert-butyl 2-oxopiperidine-1-carboxylate (45-1) (500 mg, 2.50 mmol) in THF (50 mL) was added Lithium bis(trimethylsilyl)amide (5.25 mL, 5.25 mmol) at – 78C over 30 min. After Benzyl chloroformate (712 muL, 2.50 mmol) was dissolved in THF and added to the reaction mixture at -78C stirring was continued for 2 hours. After the reaction mixture was quenched with aqueous saturated NH4Cl solution at -78C and extracted with EtOAc (2 x 100 mL), washed with brine (50 mL), dried (Na2SO4) and evaporated. The crude was purified by column chromatography (silica, gradient, 0%-20%EtOAc in Hexane as eluent) to provide 3- benzyl 1-tert-butyl 2-oxopiperidine-1,3-dicarboxylate (45-2) (605 mg) as a liquid. Yield- 90%; LC MS: ES+ 334.3.

85908-96-9, The synthetic route of 85908-96-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; C4 THERAPEUTICS, INC.; PHILLIPS, Andrew, J.; NASVESCHUK, Chris, G.; HENDERSON, James, A.; LIANG, Yanke; HE, Minsheng; LAZARSKI, Kiel; VEITS, Gesine, Kerstin; VORA, Harit, U.; (794 pag.)WO2017/197046; (2017); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Analyzing the synthesis route of 1075-89-4

As the paragraph descriping shows that 1075-89-4 is playing an increasingly important role.

1075-89-4, 8-Azaspiro[4.5]decane-7,9-dione is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 3 0.24 g of an oil dispersion of sodium hydride are washed free of oil with hexane and then suspended in 3 ml of anhydrous dimethylformamide. The solution of 0.84 g of 3,3-tetramethyleneglutarimide in 5 ml of dry dimethylformamide is added dropwise to said suspension at room temperature and the mixture is stirred for additional 30 minutes before the solution of 0.92 of 1-(2-chloroethyl)-4-diphenylmethoxypiperidine hydrochloride in 5 ml of dry dimethylformamide is added dropwise. After stirring the mixture at room temperature for 18 hours, it is poured onto 30 ml of ice water and repeatedly extracted with diethyl ether. The extract is washed successively with 1 N aqueous sodium hydroxide and brine, dried and evaporated. The residue is taken up in ethyl acetate and the solution acidified with ethereal hydrogen chloride, to yield the N-[2-(4-diphenylmethoxypiperidino)-ethyl]-beta,beta-tetramethyleneglutarimide hydrochloride, melting at 169-171; it is identical with the compound obtained according to Example 1., 1075-89-4

As the paragraph descriping shows that 1075-89-4 is playing an increasingly important role.

Reference:
Patent; Ciba-Geigy Corporation; US4261990; (1981); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Simple exploration 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

General procedure: 4-Chloro-2-(methylthio)pyrimidine-5-carbohydrazide (2.2 mmol) was heated with ethanol (10 mL) and a few drops of glacial acetic acid. Substituted aldehyde (2.2 mmol) was added on the mixture and refluxed for 4 h. The reaction was finalized by thin layer chromatography control. The precipitate was filtered, dried and purified with methanol., 10338-57-5

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

Reference:
Article; Akda?, Kadryi?Ye; Uenal, Goekhan; Tok, Fati?H; Aricio?lu, Feyza; Edi?P Temel, Hali?De; Kocyi??i?T-Kaymakcio?lu, Bedi?A; Acta poloniae pharmaceutica; vol. 75; 5; (2018); p. 1147 – 1159;,
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Analyzing the synthesis route of 768-66-1

The synthetic route of 768-66-1 has been constantly updated, and we look forward to future research findings.

768-66-1, 2,2,6,6-Tetramethylpiperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,768-66-1

Experimental Section: Preparation of the reagent TMPMgCl·LiCl (5b): ; A dry and argon flushed 250 mL flask, equipped with a magnetic stirrer and a septum, was charged with freshly titrated i-PrMgCl·LiCl (100 mL, 1.2 M in THF, 120 mmol). 2,2,6,6-tetramethylpiperidine (TMPH) (19.8 g, 126 mmol, 1.05 equiv) was added dropwise at room temperature. The reaction mixture was stirred until gas evaluation was completed (ca. 24 h) at room temperature.

The synthetic route of 768-66-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ludwig-Maximilians-Universitaet Muenchen; EP1810974; (2007); A1;,
Piperidine – Wikipedia
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Analyzing the synthesis route of 5166-67-6

As the paragraph descriping shows that 5166-67-6 is playing an increasingly important role.

5166-67-6, Ethyl N-methylpiperidine-3-carboxylate is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5166-67-6, 3-Methyl-5-(l -methylpiperidin-3-yl)-l ,2,4-oxadiazole (5c):I-N-methyl-ethyl nipecotate (4c) (0.7 g, 0.0041 mol) and acetamide oxime (0.75g, 0.0102 mol) were dissolved in 30 mL tetrahydrofuran. Sodium methoxide (l . l g, 0.0205 mol) was added and the mixture was heated at reflux for 2 hours. The mixture was concentrated to remove THF and partitioned between water (25 mL) and dichloromethane (1 x 25 mL). The aqueous layer was extracted with an additional 2 x 25 mL dichloromethane. The combined organics were washed with 1 chi 50 mL saturated sodium chloride, and dried over Na2SC>4. The dried organics were evaporated to an oil. The residue was chromatographed with 5 g silica gel, 5% methanol/ethyl acetate, to obtain 0.51 g of the free base. Hydrochloric acid in ethanol (2.5 M) (1.6 mL, 0.01 1 mol) was added and the mixture was concentrated to dryness. Crystallization from ethanol/MTBE afforded 436 mg white solid. MS (ESI) m/z 182 [M+H]+. NMR (DMSO-d6) 5 1.59- 1.66 (m, 1 H), 1.88- 1.98 (s, 2 H), 2.17-2.20 (d, 1 H), 2.34 (s, 3 H), 2.77 (s, 3 H), 2.92-2.95 (m, 1 H), 3.18-3.21 (m, 1 H), 3.37- 3.47, (d, 1H), 3.60-3.78, (m, 2H).

As the paragraph descriping shows that 5166-67-6 is playing an increasingly important role.

Reference:
Patent; MITHRIDION, INC.; ABRAHAM, Brent, D.; COPP, Richard, R.; FARNHAM, James, G.; HANSON, Seth, A.; HENDRICKSON, Michael, L.; OCKULY, Jeffrey, C.; TWOSE, Trevor, M.; VERDONE, Melinda, L.; WO2011/85406; (2011); A1;,
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Piperidine | C5H11N – PubChem

 

Simple exploration of 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.

To a solution of 2,7-diazaspiro[4.5]decan-1-one hydrochloride (1.0 g, 5.26 mmol) in DCM (10 mL), benzaldehyde (0.53 mL, 5.26 mmol) was added and the mixture was stirred at RT for 15 mm, then NaBH(OAc)3 (1.67 g, 7.89 mmol) was added and the mixture was left stirring at RT overnight. Thereaction was quenched with saturated NaHCO3 solution, then phases were separated and aqueous one was backextracted with DCM twice. Combined organics were washed with brine, dried and concentrated under reduced pressure. Crude material was purified by FC on NH column (eluent: Cy to 50% AcOEt) affording 7-benzyl-2,7-diazaspiro[4.5]decan-1-one (p139, 890 mg, y= 69%) as white solid. MS (ES) (m/z): 245.2 [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; SHIRE INTERNATIONAL GMBH; CREMONESI, Susanna; LUKER, Tim; SEMERARO, Teresa; MICHELI, Fabrizio; (257 pag.)WO2016/42452; (2016); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem