Some tips on 14813-01-5

The synthetic route of 14813-01-5 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.14813-01-5,1-Benzylpiperidin-3-ol,as a common compound, the synthetic route is as follows.

1-Benzyl-3-piperidinol (20 g), toluene (200 mL), methyl acetoacetate (24.3 g), Manganese sulfate (3.54 g) was added to a 500 mL reaction flask, heated to reflux for 6 hours, and detected by HPLC. The remaining 25.6% of 1-benzyl-3-piperidinol, plus an atmospheric distillation unit, distills off the ethanol produced by the reaction. The reaction was completed in 2 hours, cooled to 0~10 C, adjusted to a pH of about 3, and the product was extracted with water (50 mL × 2). The aqueous phases were combined and the pH of the aqueous phase was adjusted to approximately 7 and extracted with ethyl acetate (50 mL×2). The combined organic layers were washed with brine (30 mL×2) Concentrated to dryness gave a yellow oil (26.5 g)., 14813-01-5

The synthetic route of 14813-01-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tianjin Changyuan Pharmaceutical Technology Co., Ltd.; Chi Fangfei; Ying Zixiang; Liu Wenjuan; Mo Lan; (9 pag.)CN104529872; (2018); B;,
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Brief introduction of 2905-56-8

2905-56-8 1-Benzylpiperidine 76190, apiperidines compound, is more and more widely used in various fields.

2905-56-8, 1-Benzylpiperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Oxidation of various tertiary amines using catalyst B was carried out following the procedure as in example 2 and the results are given in Table 2., 2905-56-8

2905-56-8 1-Benzylpiperidine 76190, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; Council of Scientific and Industrial Research; EP1348692; (2003); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

New learning discoveries about 85908-96-9

85908-96-9 N-Boc-2-Piperidone 7577838, 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.85908-96-9,N-Boc-2-Piperidone,as a common compound, the synthetic route is as follows.,85908-96-9

Lithium bis(trimethylsilyl)amide (11.1 mL of a 1 M solution in THF, 11.1 mmol) was slowly added at 78 C underan argon atmosphere to a solution of lactam 1b (1.0 g, 5.05 mmol) in anhydrous THF (100 mL), and thesolution was stirred for 1 h. Then, ethyl chloroformate (532 l, 5.56 mmol) and, after 1 h of continuousstirring at 78 C, a solution of PhSeCl (1.48 g, 7.58 mmol) in anhydrous THF (10 mL) were addedto the solution. The mixture was stirred for a further 1 h and poured into saturated aqueous NH4Cl.The resulting mixture was extracted with EtOAc, and the combined organic extracts were dried,filtered, and concentrated under reduced pressure. Flash chromatography (8:2 hexane-EtOAc) of theresulting oil gave the seleno derivative 7 (1.79 g, 83% yield) as a yellow foam: IR (ATR Pike) (cm1):1718 (CO); 1H-NMR (300 MHz, CDCl3): d = 1.27 (t, J = 7.2 Hz, 3H, CH2CH3), 1.54 [s, 9H, (CH3)3C], 1.73(m, 1H, H-5), 1.84 (m, 1H, H-5), 2.01 (ddd, J = 13.8, 10.2, 5.7 Hz, 1H, H-4), 2.28 (dt, J = 13.8, 6.0 Hz, 1H,H-4), 3.52 (m, 1H, H-6), 3.61 (ddd, J = 13.2, 8.4, 5.4 Hz, 1H, H-6), 4.22 (qd, J = 7.2, 3.3 Hz, 2H, CH2CH3),7.31 (t, J = 7.2, 2H, HAR), 7.41 (t, J = 7.2 Hz, 1H, HAR), 7.65 (t, J = 7.2 Hz, 2H, HAR); HRMS (ESI) calcdfor [C19H25NO5Se + Na+]: 450.0787, found: 450.0788.

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

Reference:
Article; Arioli, Federica; Perez, Maria; Are, Celeste; Molins, Elies; Bosch, Joan; Amat, Mercedes; Molecules; vol. 24; 3; (2019);,
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New learning discoveries about 71985-80-3

71985-80-3 1-Methylpiperidine-4-carboxylic acid hydrochloride 2760043, apiperidines compound, is more and more widely used in various fields.

71985-80-3, 1-Methylpiperidine-4-carboxylic acid hydrochloride is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

71985-80-3, 1-Methylpiperidine-4-carboxylic acid hydrochloride salt 10 g (55.7 mmol) was added to thionyl chloride (25 ml) and stirred at room temperature until the solid dissolved completely. The reaction mixture was stirred for another 20 minutes and concentrated. The product was used for the next step without further purification. 1-Methylpiperidine-4-carboxylic acid hydrochloride salt 10 g (55.7 mmol) was added to thionyl chloride (25 ml) and resulting mixture stirred at room temperature until the solid dissolved completely. The reaction mixture was stirred for another 20 minutes and concentrated. The product was used for the next step without further purification.; EXAMPLE 5 Synthesis of N-benzhydryl-4-((4-chlorophenyl)(1-methylpiperidin-4-yl)methyl)piperazine-1-carboxamide A. Synthesis of 1-Methylpiperidine-4-carboxylic acid chloride 1-Methylpiperidine-4-carboxylic acid hydrochloride salt 10 g (55.7 mmol) was added to thionyl chloride (25 ml) and resulting mixture stirred at room temperature until the solid dissolved completely. The reaction mixture was stirred for another 20 minutes and concentrated. The product was used for the next step without further purification.

71985-80-3 1-Methylpiperidine-4-carboxylic acid hydrochloride 2760043, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; NeuroMed Technologies Inc.; US2006/63775; (2006); A1;,
Piperidine – Wikipedia
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Brief introduction of 297172-16-8

297172-16-8, 297172-16-8 (4-Methylpiperidin-4-yl)methanol 22507737, apiperidines compound, is more and more widely used in various fields.

297172-16-8, (4-Methylpiperidin-4-yl)methanol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step 4: 4-((4-methylpiperidin-4-yl)methoxy)-9-(2-trimethylsilanyl-ethoxymethyl)-9H- dipyridor2,3-b;4′,3′-dlpyrrole-6-carbonitrileTo a solution of (4-methylpiperidin-4-yl)methanol (989 mg, 7.7 mmol) in 1,4-dioxane (18 mL) and N,N-dimethylformamide (12 mL) was added sodium hydride as 60% dispersion in mineral oil (670 mg, 28 mmol). The reaction mixture was stirred at ambient temperature for 5 minutes before 4-chloro-9-(2-trimethylsilanyl-ethoxymethyl)-9H- dipyrido[2,3-b;4′,3′-d]pyrrole-6-carbonitrile (428 mg, 1.2 mmol) was added in one portion and the reaction mixture was heated at 40C for 18 hours. The cooled reaction mixture was diluted with water (20 mL) and ethyl acetate (50 mL). The organic layer was separated, dried over sodium sulfate, filtered, concentrated in vacuo, and purified flash chromatography (silica, 40 g, ISCO, 1-20% methanol in methylene chloride) to afford the title compound as an off-white solid, which was used in the next step without any further purification (300 mg, 56%).

297172-16-8, 297172-16-8 (4-Methylpiperidin-4-yl)methanol 22507737, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; DYKE, Hazel Joan; GAZZARD, Lewis J.; WILLIAMS, Karen; WO2011/73263; (2011); A1;,
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Brief introduction of 5166-67-6

As the paragraph descriping shows that 5166-67-6 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.5166-67-6,Ethyl N-methylpiperidine-3-carboxylate,as a common compound, the synthetic route is as follows.

5166-67-6, A solution of (R)-ethyl 1-methylpiperidine-3-carboxylate (5.69 g, 33 mmol) in ether (20 ml) was added dropwise to a stirred solution of lithium aluminum hydride (36.6 ml of a 1M solution in THF, 36.6 mmol) in ether (85 ml) cooled to maintain a reaction temperature of 20 C. The mixture was stirred for 1.5 hours at ambient temperature and then water (1.4 ml), 15% aqueous sodium hydroxide solution (1.4 ml) and then water (4.3 ml) were added. The insolubles were removed by filtration and the volatiles removed from the filtrate by evaporation to give (R)-(1-methylpiperidin-3-yl)methanol (4.02 g, 94%) as a colourless oil. 1H NMR Spectrum: (DMSOd6) 1.06(q, 1H); 1.51-1.94(m, 5H); 2.04(s, 3H); 2.34(br s. 1H); 2.62(m, 1H); 2.78(d, 1H); 3.49(m, 1H); 3.59(m. 1H); MS-ESI: 130 [MH]+.

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

Reference:
Patent; Zeneca Limited; Zeneca Pharma S.A.; US6414148; (2002); B1;,
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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

A solution of 2,2,6,6-tetramethyl-4-piperidine (TMP) (45 mL, 267 mmol) in THF (400 mL) was cooled to -78 C. under an atmosphere of nitrogen. n-Butyl lithium (2.5 M in hexane, 110 mL, 275 mmol) was added slowly maintaining the temperature below -70 C. After addition, the reaction mixture was warmed to -50 C. and stirred for 30 minutes. The clear solution became turbid indicating the salt formation. The reaction mixture was recooled to -80 C., and a solution of 2-fluoro-4-methylbenzonitrile (32.4 g, 240 mmol) in THF (150 mL) was slowly added maintaining temperature below -70 C. The mixture was then warmed to -50 C. and stirred for 30 minutes. The mixture was recooled to -70 C. and a saturated solution of iodine (67 g, 264 mmol) in THF (150 mL) was added slowly maintaining the temperature at -70 C. After addition, the mixture was warmed to ambient temperature. The reaction mixture was poured into a solution of Na2S2O3 (160 g in 1.5 L of water) and stirred for 1 h. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with brine, dried over Na2SO4, and filtered. The volatiles were evaporated under reduced pressure. The crude product was subjected to vacuum distillation, and at about 60 C., the excess TMP was removed, at about 100 C., the starting compound 2-fluoro-4-methylbenzonitrile and a small amount of 2-fluoro-3-iodo-4-methylbenzonitrile were removed and, finally at 115 C., pure 2-fluoro-3-iodo-4-methylbenzonitrile was obtained as an off-white amorphous solid. MS (ESI, pos. ion) m/z: 261.9 (M+1).

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

Reference:
Patent; Amgen Inc.; US2006/199817; (2006); A1;,
Piperidine – Wikipedia
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Simple exploration of 20691-89-8

20691-89-8 1-Methyl-4-piperidinemethanol 271971, 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.20691-89-8,1-Methyl-4-piperidinemethanol,as a common compound, the synthetic route is as follows.,20691-89-8

(1-Methyl-piperidin-4-yl)-methanol (2. 5USD g, 20 mmol) and hydroxy-diphenyl-acetic acid methyl ester (9. 69 g, 40 mmol) are suspended in toluene (65 ml). Molecular sieve 4A (1 g) is added and the mixture is stirred at room temperature for 10 minutes. Sodium (0.08 g) is added and the reaction mixture stirred at 80OC for 3 hours. Additional sodium (0.1 g) is then added and heating maintained at 80OC for 18 hours. The reaction mixture is cooled to room temperature, solid filtered off, and washed with ethylacetate. The filtrate is washed once with saturated aqueous NAHCO3 solution (50 ml) and twice with aqueous HCL 1M (25 ml each). The combined acidic aqueous layers are basified with saturated aqueous NAHCO3 solution and solid NAHCO3, the resulting precipitate is removed by filtration, drying under vacuum gives the title product as a white solid (M+H) + : 340.09.

20691-89-8 1-Methyl-4-piperidinemethanol 271971, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2005/815; (2005); A2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Some tips on 10338-57-5

As the paragraph descriping shows that 10338-57-5 is playing an increasingly important role.

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: To a solution of various alpha,beta-unsaturated ketones 9 (0.28mmol) and different benzaldehydes (0.3mmol) in EtOH (5mL) at room temperature was added dropwise a solution of 20% NaOH. The reaction mixture was stirred at room temperature overnight and the resulting mixture was diluted with H2O (15mL) and extracted with EtOAc. The combined organic layers were washed with brine (15mL) and dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure. The residue was further purified by chromatography on silica gel to afford target Asymmetric MACs 10a-c., 10338-57-5

As the paragraph descriping shows that 10338-57-5 is playing an increasingly important role.

Reference:
Article; Liu, Zhiguo; Tang, Longguang; Zou, Peng; Zhang, Yali; Wang, Zhe; Fang, Qilu; Jiang, Lili; Chen, Gaozhi; Xu, Zheng; Zhang, Huajie; Liang, Guang; European Journal of Medicinal Chemistry; vol. 74; (2014); p. 671 – 682;,
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Downstream synthetic route of 20691-89-8

As the paragraph descriping shows that 20691-89-8 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.20691-89-8,1-Methyl-4-piperidinemethanol,as a common compound, the synthetic route is as follows.

Example 3b An alternative method of preparation is as follows: Triphenylphosphine (615mg, 2.3mmol) followed by diethyl azodicarboxylate (369mul, 2.3mmol) were added to a solution of 4-hydroxymethyl-1-methylpiperidine (151mg, 1.1mmol), (J Med. Chem 1973, 16, 156), and 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (250mg, 0.78mmol), (prepared as described for the starting material in Example 7), in methylene chloride (5ml). After stirring for 30 minutes at ambient temperature, 4-hydroxymethyl-1-methylpiperidine (51mg, 0.39mmol), triphenylphosphine (102mg, 0.39mmol) and diethyl azodicarboxylate (61mul, 0.39mmol) were added. After stirring for 15 minutes, the volatiles were removed under vacuum and the residue was purified by column chromatography eluding with methylene chloride/acetonitrile/methanol (70/10/20 followed by 75/5/20 and 80/0/20). The fractions containing the expected product were combined and the volatiles were removed by evaporation. The residue was dissolved in a mixture of methylene chloride and methanol and 5M hydrogen chloride in isopropanol was added. The suspension was concentrated and the solid was collected by filtration, washed with ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline hydrochloride (16mg, 4%)., 20691-89-8

As the paragraph descriping shows that 20691-89-8 is playing an increasingly important role.

Reference:
Patent; AstraZeneca AB; EP1244647; (2006); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem