Tag: M.W:100-200

14813-01-5, 1-Benzylpiperidin-3-ol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Then, 11.8 g of the 1-benzyl-3-hydroxypiperidine and 5.6 g of diketene were reacted similarly as in Reference Example 1, and the reaction product was purified by silica gel column chromatography (eluent:chloroform:methanol=9:1 v/v), to obtain 10.65 g of acetoacetic acid-N-benzyl-3-piperidinyl ester (yield: 62.5%). This was used in the reaction of Example 4 without distillation. NMR spectrum (CDCl3, delta): 1.30-1.90(4H, broad), 2.10-2.95(4H, broad), 2.27(3H, s), 3.43(2H, s), 3.54(2H, s), 4.73-5.2(1H, broad), 7.30(5H, s)

14813-01-5, 14813-01-5 1-Benzylpiperidin-3-ol 85773, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; Kyowa Hakko Kogyo Co., Ltd.; US4448964; (1984); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.768-66-1,2,2,6,6-Tetramethylpiperidine,as a common compound, the synthetic route is as follows.

EXAMPLE 1 Preparation of (2,2,6,6-tetramethyl-piperidine) N-oxide (TEMPO) An organic solution consisting of 5 g of 2,2,6,6-tetramethylpiperidine (i.e. 0.0354 mol) dissolved in 20 ml of dichloromethane is prepared with stirring in a 100 ml round-bottomed flask fitted with 2 dropping funnels, a condenser, a pH-measuring probe and a stirrer. 20 ml of water are then added to this solution so as to have a two-phase system. Next, 10.8 g of a 40% solution of peracetic acid 4n acetic acid and aqueous 35% by weight K2CO3 solution are introduced (with stirring) slowly and simultaneously. The molar amount of peracetic acid introduced is 0.0568 mol, which corresponds to a peracetic acid/amine molar ratio of 1.6. The amount of aqueous K2CO3 solution is adjusted such that the pH of the aqueous phase of the two-phase medium is maintained at between 7.2 and 7.5 in the course of the addition. 20 minutes after the addition, the total disappearance of the amine and the formation of TEMPO are found by gas chromatography (GC). The reaction is stopped and K2CO3 solution is added so as to obtain a pH equal to 9, and the red-colored TEMPO is then extracted with CH2Cl2. Evaporation of the solvent gives 4.9 g of TEMPO with a melting point equal to 36 C. The purity of the TEMPO is checked by GC relative to a sample of pure product (purity greater than 99%) sold by the company Aldrich. Mass spectrum (m/e): 157 (M+1), 768-66-1

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

Reference：
Patent; Atofina; US6538141; (2003); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

86542-94-1, 1-(Piperidin-4-yl)propan-1-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of Intermediate I (1.1 g, 3.1 mmol) in EtOH (15 mL) was added l-Piperidin-4-yl-propan-l- one (437 mg, 3.1 mmol) and DIEA (1.55 g, 12 mmol). The mixture was stirred at 80 C for 3 hours then the mixture was evaporated to dryness. The crude product was purified by silica gel chromatography eluted with PE: EA =(10:1) to give desired product (0.95 g). MS (m/e): 454 (M + H)+ NMR (MeOD) delta, 8.55 (s, 1H), 7.65-7.74 (m, 2H), 7.56-7.63 (m, 2H), 7.46-7.54 (m, 2H), 7.42-7.44 (m, 2H), 7.36-7.38 (m, 1H), 4.50-4.80 (m, 2H), 4.23-4.60 (m5 2H),3.64-4.12 (m, 2H), 3.36-3.60 (m, 1H), 2.70-3.12 (m, 3H), 2.23-2.69 (m, 2H), 1.64-2.17 (m, mH), 1.16-1.56 (m, 1H), 0.64-1.15 (m, 3H).

86542-94-1, As the paragraph descriping shows that 86542-94-1 is playing an increasingly important role.

Reference：
Patent; MERCK SHARP & DOHME CORP.; COBURN, Craig; WANG, Jiabing; SANTARELLI, Vince; HU, Shuangxi; CUI, Mingxiang; HU, Bin; DONG, Jingchao; LUO, Yunfu; SOLL, Richard, M.; WO2011/106276; (2011); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.138377-80-7,3-Aminopiperidin-2-one hydrochloride,as a common compound, the synthetic route is as follows.

138377-80-7, Reference Example 1: 3-(Benzoylamino)tetrahydropyridin-2-one:; 3-aminotetrahydropyridin-2-one hydrochloride (10 mmol) and K2C03 (30 mmol) were added to water (20 mL) and stirred. A solution of benzoyl chloride (10 mmol) in CH2C12 (10 mL) was added and the reaction was stirred overnight at room temperature in an inert atmosphere (using dinitrogen). The reaction was extracted with CH2C12 (3 chi 50 mL), and the combined organic layers where then dried (Na2S04) and reduced in vacuo to give a crude product which was recrystallised from CH2C12 / petroleum ether (bp 40-60 °C) to give the product (1.62 g, 74percent): Vmax/cm”1 3250 (N-H, amide), 1664, 1633, 1538 (secondary CONH, lactam), 1605, 1578, 1486 (aromatic ring), 766, 715, 704, 690 (monosubstituted benzene ring). NMR: deltaEta (400MHz, CDC13) 7.80 (2H, br d, J 7.0, ortho-H), 7.47-7.40 (1 H, m, para-U), 7.42-7.39 (1 H, m, C6H5-CONH), 7.40-7.31 (2H, m, meta-W), 6.78 (1 H, br s, CONH-CH2), 4.41 (1 H, dt, J 1 1.5, 5.5, CH-CO), 3.36-3.23 (2H, m, CH2NH), 2.59 (1 H,22P66854. WOO L Spec as Hied 8.06.1 1 dq, J 13.0, 4.5, NHCH-CH;), 1.94-1.81 (2H, m, lactam CH2), 1.64 (IH, tt, J 12.5, 8.0, NHCH-CH^).13C NMR: 5C (100MHz, CDC13) 171.9 (lactam C=0), 167.4 (aryl C=0), 134.0 (ipso- C), 131.4 (ortho-C), 128.3 (meta-C), 127.0 (para-C), 50.8 ( H-CO), 41.5 (CH2NH), 27.0 (lactam CH2), 20.9 (lactam CH2).HRMS (+ESI) Ci2H,4N202 + Na+: calcd 241.0947; found 241.0950.

As the paragraph descriping shows that 138377-80-7 is playing an increasingly important role.

Reference：
Patent; CAMBRIDGE ENTERPRISE LIMITED; FUNXIONAL THERAPEUTICS LIMITED; GRAINGER, David, John; FOX, David John; WO2011/154696; (2011); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

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 2b (1.75 g, 10 mmol) and triethyl 4-phosphonocrotonate (3.3 mL, 15 mmol) in THF (40 mL), sodium hydride (60% dispersion in mineral oil, 800 mg, 20 mmol) was carefully added at 0 C under Ar. After the reaction mixture was stirred at ambient temperature for 3 h, the reaction was quenched by adding ethanol (1 mL) and water (20 mL), and the product was extracted with EtOAc (3 x 20 mL). The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc [4:1]) to give 3b (1.9 g, 7.0 mmol, 70%) as yellow crystals., 10338-57-5

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

Reference：
Article; Kiyama, Masahiro; Iwano, Satoshi; Otsuka, Satoshi; Lu, Shijia W.; Obata, Rika; Miyawaki, Atsushi; Hirano, Takashi; Maki, Shojiro A.; Tetrahedron; vol. 74; 6; (2018); p. 652 – 660;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

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

2) Experimental Procedures and Analytical DataTypical Procedure 1: Preparation of the reagent TMPZnCl.LICl (2):A dry and argon flushed 250 mL Schlenk-flask, equipped with a magnetic stirrer and a septum, was charged with freshly 2,2,6,6-tetramethylpiperidine (10.22 mL, 60 mmol) dissolved in THF (60 mL). This solution was cooled to -40 C. and n-BuLi (2.4 M in hexane, 25 mL, 60 mmol) was dropwise added. After the addition was complete, the reaction mixture was allowed to warm up slowly to -10 C. for 1 h. ZnCl2 (1.0 M in THF, 66 mL, 66 mmol) was dropwise added and the resulting solution was stirred for 30 min at -10 C. and then for 30 min at 25 C. The solvents were then removed under vacuum affording a yellowish solid. Freshly distilled THF was then slowly added under vigorous stirring until the salts were completely dissolved. The freshly prepared TMPZnCl.LiCl (2) solution was titrated prior to use at 25 C. with benzoic acid using 4-(phenyiazo)diphenylamine as indicator. A concentration of 1.3 M in THF was obtained.Typical Procedure for the Zincation of Polyfunctionalized Aromatics and Heterocycles with TNIPZnCl.-LICl (TP 2):

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

Reference：
Patent; Knochel, Paul; Mosrin, Marc; US2011/288296; (2011); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

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.

General procedure: Appropriate benzaldehyde (10 mmol) was dissolved in ethanol (20 mL). Sodium metabisulfite (15 mmol) in 5 mL water was added in portion over 5 min. The reaction mixture was stirred at room temperature for 1 h and subsequently stirred at 4 C overnight. The precipitate formed was filtered and dried to afford sodium bisulfite adducts (55%-90%).

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

Reference：
Article; Yoon, Yeong Keng; Ali, Mohamed Ashraf; Wei, Ang Chee; Choon, Tan Soo; Ismail, Rusli; European Journal of Medicinal Chemistry; vol. 93; (2015); p. 614 – 624;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

280774-03-0, (1-Isopropylpiperidin-4-yl)methanol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Reference Example 2 Oxalyl chloride (3.15 ml) was dissolved in 30 ml of dichloromethane, a solution of 3.20 ml of dimethyl sulfoxide in 6 ml of dichloromethane was added thereto at-70?C, the mixture was stirred for 15 minutes, a solution of 2.93 g of (1-isopropyl-4-piperidyl)methanol in 15 ml of dichloromethane was added thereto at -70?C and the mixture was stirred for 1 hour. After 12.5 ml of triethylamine were added at -70?C, the mixture was raised to room temperature, then water and a saturated aqueous solution of sodium hydrogen carbonate were added and the mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate, the solvent was evaporated in vacuo and ethyl acetate was added to the resulting residue. After removing the insoluble matter by filtration, the solvent was evaporated in vacuo to give 1.15 g of 1-isopropylpiperidine-4-carbaldehyde. This compound was used for the next reaction without purification.

280774-03-0, 280774-03-0 (1-Isopropylpiperidin-4-yl)methanol 11147855, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; YAMANOUCHI PHARMACEUTICAL CO. LTD.; EP1336605; (2003); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

138377-80-7, 3-Aminopiperidin-2-one hydrochloride is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

24.64 mg of 4 (0.087 mmol), 41.05 mg of sodium 2-ethyl-hexanoate (0.247 mmol), 20.16 mg of 15 (which may be prepared according to the procedures described in WO 2002/081480, and the content of which is incorporated herein by reference) (0.134 mmol) and 2 ml of THF are successively introduced into a 20 ml round-bottomed flask with stirring and under an argon atmosphere. Stirring is continued for 4 days at r.t. 20 ml of EtOAc are added to the reaction medium, which is then washed successively with 20 ml of NaOH solution (0.1 N), 20 ml of water and 20 ml of saturated NaCl solution. As product has visibly dissolved in the aqueous phase, this aqueous phase is extracted twice with a mixture of 50 ml of CH2Cl2 and 5 ml of MeOH. The 3 organic phases are combined, dried, filtered and then evaporated to dryness. The crude product is purified by PCC with a 93/7 CH2Cl2/MeOH mixture. 28.49 mg of product 16 are collected (Yld=83percent). TLC (90/10 CH2Cl2/MeOH): Rf=0.28 1H NMR (400 MHz, CDCl3): delta (ppm)=7.11 (d, 1H); 5.70 (d, 1H); 5.67 (m, 1H); 5.48 (dd, 1H); 4.72 (m, 1H); 4.20 (d, 1H); 4.02 (d, 1H); 3.80 (d, 1H); 3.50 (s, 1H); 3.49 (s, 3H); 3.36 (m, 2H); 2.54 (m, 2H); 1.96 (m, 2H); 1.47 (s, 6H); 1.02 (s, 9H) LCMS (ES+, 30 V): tR=2.92 mn|m/z=797+ (2M+H+); 399+ (M+H+); 341+ (M+H+[(H3C)2CO]); 841 (2 MH+HCOOH); 443 (MH+HCOOH), 138377-80-7

138377-80-7 3-Aminopiperidin-2-one hydrochloride 19795138, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; AVENTIS PHARMA S.A.; US2007/244087; (2007); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

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.

10338-57-5, General procedure: For the reactions, 4-piperidinone or corresponding ketones (1 mmol) and 2-bromobenzaldehyde or corresponding aldehydes(2.5 mmol) were dissolved in ethanol (10 mL). The mixture wasrefluxed at 78 C and added with 0.5 mL 40% NaOH or AcOH/HCl.Reactions were monitored by TLC, when the reactions were accomplished, cooled on ice. The products could precipitate or be purified by crystallization and column chromatography using PE/EA as the eluent. Among these compounds, A4, A6, C5, D1, D2, D3 and D4 were unreported.

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

Reference：
Article; Jin, Rong; Chen, Qiuxiang; Yao, Song; Bai, Encheng; Fu, Weitao; Wang, Ledan; Wang, Jiabing; Du, Xiaojing; Wei, Tao; Xu, Haineng; Jiang, Chengxi; Qiu, Peihong; Wu, Jianzhang; Li, Wulan; Liang, Guang; European Journal of Medicinal Chemistry; vol. 144; (2018); p. 218 – 228;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem