Day: March 24, 2022

1187173-43-8, 2,7-Diazaspiro[4.5]decan-1-one hydrochloride is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2,7-Diazaspiro[4.5]decan-1 -one hydrogen chloride (80 mg, 0.420 mmol) was dissolved in dichloromethane (4 mL) and triethylamine (0.1 17 mL, 0.839 mmol) before the addition of 3-(trifluoromethyl)benzenesulfonyl chloride (1 13 mg, 0.462 mmol). After stirring for 20 h the reaction mixture was concentrated in vacuo and the resulting residue was purified by MDAP to give 7-{[3-(trifluoromethyl)phenyl]sulfonyl}- 2,7-diazaspiro[4.5]decan-1 -one (60 mg, 0.162 mmol, 39% yield) as a white solid. 1 H NMR (400 MHz, DMSO-d6) delta ppm 1 .35 – 1.46 (m, 2 H) 1.51 – 1.64 (m, 1 H) 1.66 – 1 .74 (m, 1 H) 1.90 – 1.98 (m, 1 H) 2.00 – 2.09 (m, 1 H) 2.20 – 2.31 (m, 2 H) 3.12 – 3.24 (m, 2 H) 3.37 (d, J=1 1 .40 Hz, 1 H) 3.67 (d, J=1 1 .24 Hz, 1 H) 7.76 (s, 1 H) 7.92 (t, J=7.87 Hz, 1 H) 7.98 (s, 1 H) 8.08 (d, J=7.95 Hz, 1 H) 8.14 (d, J=7.84 Hz, 1 H). MS ES+ve m/z 363 (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
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: The 4-alkyl(aryl)aminobenzaldehyde (1 mmol) was added to(RMe2Si)3CLi, R=H,Me (1 mmol) in THF under argon. The mixturewas reacted according to Tables 1 and 2. The reaction was quenchedwith H2O, extracted with CH2Cl2 and dried over Na2SO4. The solventwas evaporated under reduced pressure and the residue was purifiedby preparative column chromatography (n-hexane/ethylacetate) andthe corresponding products were obtained.

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

Reference：
Article; Safa, Kazem Dindar; Nadimi, Sanaz; Alyari, Maryam; Journal of Chemical Research; vol. 38; 8; (2014); p. 498 – 501;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.142851-03-4,Ethyl N-Boc-piperidine-4-carboxylate,as a common compound, the synthetic route is as follows.

To a solution of 1-tert-butyl 4-ethyl piperidine-1,4-dicarboxylate (2.00 g, 7.77 mmol) in EtOH (26 mL) was added hydrazine hydrate (5.84 g, 117 mmol) at room temperature. The reaction mixture was refluxed overnight, cooled to room temperature and concentrated in vacuo. The residue was dissolved in DCM, washed with water 3 times and brine, dried over Na2SO4, filtered and concentrated in vacuo to afford tert-butyl 4-(hydrazinecarbonyl)piperidine-1-carboxylate (985 mg, 52%) as a white solid. 1H-NMR (CDCl3, Varian, 400 MHz): delta 1.46 (9H, s), 1.58-1.70 (2H, m), 1.73-1.85 (2H, m), 2.19-2.26 (1H, m), 2.27 (2H, br. s), 3.90 (2H, s), 4.15 (2H, br. s), 6.99 (1H, s).

142851-03-4, As the paragraph descriping shows that 142851-03-4 is playing an increasingly important role.

Reference：
Patent; HANDOK INC.; CMG Pharmaceutical Co., Ltd.; Kim, Moonsoo; Lee, Chaewoon; Lee, Gilnam; Yoon, Cheolhwan; Seo, Jeongbeob; Kim, Jay Hak; Lee, Minwoo; Jeong, Hankyul; Choi, Hyang; Jung, Myung Eun; Lee, Ki Nam; Kim, Hyun Jung; Kim, Hye Kyoung; Lee, Jae Il; Lee, MinWoo; Kim, Misoon; Choi, Soongyu; (124 pag.)US2016/168156; (2016); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

20691-89-8, 1-Methyl-4-piperidinemethanol is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 57 ; 3-methoxv-4-I(I -methvlDiDeridin-4-Vl)methoxvlbenzonitrile; 53.3 ml of 1 N sodium bis (trimethylsilyl)amide added to a stirred solution of 6.63 g (51.3 mmol) of (1-methyl-piperidin-4-yl)-methanol in 14 ml of THF. After 20 minutes, solid 4-fluoro-3-methoxy benzonitrile was added. The mixture was refluxed for 20 minutes, cooled to room temperature and poured into water. The mixture was extracted with ethyl acetate. The organic extracts were dried over magnesium sulfate. The solvent was removed and the residue was recrystallized from ethyl acetate-hexanes yielding 8.9 g of the title compound as a white solid: mass spectrum (electrospray, m/e): M+H 261.2.

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

Reference：
Patent; WYETH; WO2005/115145; (2005); A2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.885279-92-5,1-Boc-1,8-diaza-spiro[4.5]decane,as a common compound, the synthetic route is as follows.

8-Benzyl 1-fetaut-butyl L8-diazaspiror4.5″|decane-l,8-dicarboxylate (C-I); To a solution of 5.0 g (20.8 mmol) A-S in 200 mL CH2Cl2 cooled to 00C was added 7.3 mL (41.6 mmol) DIPEA and 3.1 mL (21.8 mmol) benzyl chloroformate. After 30 minutes, the cooling bath was removed and the reaction was stirred at room temperature for 3 h before being dumped into 0.5 M HCl in a separatory funnel. The layers were separated, the aqueous layer was extracted once with CH2Cl2, the combined organic layers were washed again with 0.5M HCl, then with saturated aqueous NaHCO3, water, dried over Na2SO4, and concentrated by rotary evaporation. The residue was purified by column chromatography on silica gel (EtOAc/hexanes) to provide C-I as a white solid. Data for C-I: LC/MS: rt = 2. 73 min; m/z (M + H) = 375.1, found; 375.2 required., 885279-92-5

885279-92-5 1-Boc-1,8-diaza-spiro[4.5]decane 34178602, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; MERCK & CO., INC.; WO2007/25069; (2007); A2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

13096-31-6, 5-Hydroxypiperidine-2-carboxylic acid is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The upper step of the product (365.22g, 2 . 516 muM, 1 . 0eq.) dissolved in MeOH (3000 ml) in. under the ice-bath adds by dropsSOCl2(448.99g, 3.774mol, 1.5eq.)dropping process temperature can be raised to reflux, then completing, reflux 2h. LC – Ms detection reaction is complete; reducing pressure and solvent, a brown yellow liquid 489.81g, yield (theoretical): 100%. The crude product directly into the next step., 13096-31-6

13096-31-6 5-Hydroxypiperidine-2-carboxylic acid 151730, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; Nanjing Furun Cade Biological Medicine Co., Ltd; Shi, Xiang; Liu, Guihua; Lian, Huawen; (18 pag.)CN106045999; (2016); 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.25137-01-3,(R)-Ethyl piperidine-3-carboxylate,as a common compound, the synthetic route is as follows.

25137-01-3, A mixture of 2-(3-(3-methylphenyl)-3-phenyl-2-propen-1-yl-oxy)ethanol (16 g, 60 mmol) and triethylamine (15.1 g, 149 mmol) in dry toluene (75 ml) kept under a nitrogen atmosphere was cooled to 5 C. and a solution of methanesulphonyl chloride (13.7 g, 119 mmol) in dry toluene (75 ml) was added dropwise keeping the temperature below 10 C. When addition was complete the reaction mixture was stirred for 1.5 h at 5 C. Water was added (100 ml) and the mixture was stirred at room temperature for 0.5 h. The phases were separated and the aqueous phase was extracted with a small portion of toluene. The combined organic extracts was washed with brine, dried (Na2SO4) and filtered. To the filtrate was added ethyl (R)-3-piperidinecarboxylate (10.3 g, 66 mmol) and potassium carbonate (9.9 g, 72 mmol) and the mixture was heated at reflux temperature for 6 days. Another portion of ethyl (R)-3-piperidinecarboxylate (5.3 g) was added and the mixture was heated at reflux temperature for another 24 h. The reaction mixture was poured into ice water (200 ml) and extracted with ethyl acetate (2*200 ml). The combined organic extracts was washed with a sodium citrate buffer solution (2*100 ml, pH 5) and then extracted with a 5% aqueous citric acid solution (4*30 100 ml). Toluene (120 ml) was added to the combined acidic extracts and sodium hydroxide pellets was added to the mixture until the pH was measured at 8.5. The phases were separated and the organic phase was dried (Na2SO4). The solvent was evaporated in vacuo to give 9.4 g (39 %) of (R)-N-(2-(3-(3-methylphenyl)-3-phenyl-2-propen-1-yloxy)ethyl)-3-piperidinecarboxylic acid ethyl ester as an oil. TLC: rf=0.50 (SiO2; dichloromethane/methanol/acetic acid=20:2:1).

As the paragraph descriping shows that 25137-01-3 is playing an increasingly important role.

Reference：
Patent; Novo Nordisk A/S; US6174898; (2001); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.61995-20-8,Benzyl 3-oxopiperidine-1-carboxylate,as a common compound, the synthetic route is as follows.,61995-20-8

To a solution of benzyl 3-oxopiperidine-1-carboxylate (30 g, 129 mmol) inMeOH (130 mL) and H20 (l7OmL) was added (NH4)2C03 (24.8 g,258 mmol) and KCN (16.7g, 258mmo1). The solution was stirred at 40 C in a sealed tube for 48 h,and then the resulting solid was filtered and washed with water(1 L). The benzyl 2,4-dioxo- 1,3 ,7-triazaspiro [4.51 decane7-carboxylate was obtained and dried in vacuo.1H NMR (400 MHz, CD3OD) 3 7.35 (br. s.,5H),5.14 – 5.07 (m, 2H), 4.60 (br. s., 1H), 3.84 (br. s., 1H), 3.49 – 3.34 (m,1H), 3.25 – 3.10 (m, 1H),2.20 – 1.93 (m, 1H), 1.92 – 1.53 (m, 3H) ppm.

As the paragraph descriping shows that 61995-20-8 is playing an increasingly important role.

Reference：
Patent; MERCK SHARP & DOHME CORP.; LIU, Jian; KOZLOWSKI, Joseph; KIM, Ronald; GAO, Xiaolei; BOGA, Sobhana Babu; YU, Younong; WU, Hao; LIU, Shilan; YANG, Chundao; (102 pag.)WO2016/164284; (2016); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

149554-03-0, tert-Butyl 2-(4-oxopiperidin-1-yl)acetate is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of Example 1.2.7 (0.055 g,), tert-butyl 2-(4-oxopiperidin-1-yl)acetate (0.014 g) and sodium triacetoxyborohydride (0.019 g) was stirred in dichloromethane (0.5 mL) at room temperature. After stirring for 2 hours, trifluoroacetic acid (0.5 mL) was added to the reaction, and stirring was continued overnight. The reaction was concentrated, dissolved in N,N- dimethylformamide (1.5 mL) and water (0.5 mL) and purified by reverse phase HPLC using a Gilson system, eluting with 10-80% acetonitrile in water containing 0.1% v/v trifluoroacetic acid. The desired fractions were combined and freeze-dried to provide the title compound. 1H NMR (501 MHz, dimethyl sulfoxide-d6) delta ppm 12.85 (s, 1H), 8.80 (s, 2H), 8.03 (d, 1H), 7.80 (d, 1H), 7.62 (d, 1H), 7.55-7.41 (m, 3H), 7.36 (q, 2H), 7.29 (s, 1H), 6.96 (d, 1H), 4.96 (s, 2H), 4.07 (s, 2H), 3.89 (t, 2H), 3.83 (s, 2H), 3.66-3.55 (m, 4H), 3.30 (s, 1H), 3.08 (s, 4H), 3.02 (t, 2H), 2.22 (d, 2H), 2.10 (s, 3H), 1.97-1.78 (m, 2H), 1.44 (s, 2H), 1.31 (q, 4H), 1.20-0.96 (m, 6H), 0.87 (s, 6H). MS (ESI) m/e 887.3 (M+H)+., 149554-03-0

As the paragraph descriping shows that 149554-03-0 is playing an increasingly important role.

Reference：
Patent; ABBVIE INC.; BENATUIL, Lorenzo; BRUNCKO, Milan; JUDD, Andrew, S.; LI, Yingchun; MCCLUSKEY, Andrew; PHILLIPS, Andrew, C.; PHILLIPS, Darren, C.; SEAGAL, Jane; SOUERS, Andrew, J.; (808 pag.)WO2017/214462; (2017); A2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.23499-01-6,1-(4-Nitrophenyl)piperidin-4-one,as a common compound, the synthetic route is as follows.

In a 500 mL three-necked flask equipped with mechanical stirrer and oil bath, the toluene solution(about 400 mL) containing virtually 120.5 g intermediate(VI), 80 mL triethyl amine, 5.3 g dimethylaminopyridine(DMAP) are added. Under stirring at 25-30 0C, 57 mL acetic anhydride are added in 30 min. It is stirred at 25 0C for2.5 hours. Once the conversion was complete (monitored byGC analysis) , the mass is quenched by adding about 30 mL of 5% sodium bicarbonate aqueous solution. The phases are divided, and the organic phase is washed with 2×20 mL of5% sodium bicarbonate aqueous solution. The combined aqueous phases are washed with 3×100 mL toluene. Finally, the combined organic phases are washed with 20 ml water. The organic phase is concentrated under reduced pressure. The obtained residue is taken up with 280 mL MTBE. It is heated to complete dissolution, then it is cooled at T. A. and then at 10 0C by stirring for 2 hours. The obtained crystal (the possible trans diastereoisomer remains almost completely dissolved in the mother liquors) is filtered off by washing with 2×30 mL of cold MTBE. The reaction is dried at 35 0C in a ventilated oven, thus obtaining 95 g of product as a white crystal. Total yield (3 steps) = 65.3%, equal to an average yield for each step of about 87%. GC titre: 99.7% (A%) ; trans diastereoisomer, about 0.02%.

23499-01-6, As the paragraph descriping shows that 23499-01-6 is playing an increasingly important role.

Reference：
Patent; F.I.S. FABBRICA ITALIANA SINTETICI S.p.A.; MOTTERLE, Riccardo; ARVOTTI, Giancarlo; BERGANTINO, Elisabetta; CASTELLIN, Andrea; FOGAL, Stefano; GALVAGNI, Marco; WO2010/100215; (2010); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem