Month: May 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3022-15-9,Piperazine-2-carboxylic acid dihydrochloride,as a common compound, the synthetic route is as follows.

Pyrazine-2-carboxylic acid hydrochloride (2 g, 9.8 mmol)And (Boc) 2O (8.6 g, 39.4 mmol)Was dissolved in THF (40 mL) and water (40 mL)Sodium bicarbonate (8.31 g, 79.8 mmol) was added,The reaction mixture was stirred magnetically at room temperature for 4 hours and then added with ethyl acetate.Poured into a separatory funnel, and the separated organic phase was washed with saturated brine, dried over anhydrous sodium sulfate,The solvent was concentrated under reduced pressure and purified by silica gel column chromatography to obtain 2.5 g of 1,4-di-tert-butoxycarbonylpiperazine-2-carboxylic acid (13-2) in a yield of 78%

3022-15-9, 3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Fujian Jinle Pharmaceutical Technology Co., Ltd.; Zhou Zhongxiang; Xing Yuanyuan; Chen Yingzhong; Deng Chengjun; Deng Honggui; Xue Wanhua; Zhang Shuzu; Chen Weipeng; Li Fang; (27 pag.)CN107174584; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.13484-40-7,1-(2-Methoxyethyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: To a solution of 6 or 7 (0.68-0.74 mmol) in 3 mL of n-BuOH kept in a PV with stirring, cyclic amines (1.02-1.11 mmol) was added. The sealed PV was placed in an oil bath at 145-150 C and stirred for 50-60 min. The solvent was evaporated in vacuo with the aid of DCM and the residue was re-dissolved in 2:1 EtOAc/DCM and washed successively with saturated NaHCO3 and NaCl solution (1 x 15 mL), respectively. The aqueous layer was washed with EtOAc (3 x 5 mL) and the organic layer was dried over anhydrous MgSO4 then filtered. The solution was evaporated in vacuo and purified using silica gel column chromatography with appropriate eluents (EtOAc/hexanes 3:1 and 1:3 v/v, respectively or 9:1 DCM/EtOAc) to afford either solid or semisolid products., 13484-40-7

As the paragraph descriping shows that 13484-40-7 is playing an increasingly important role.

Reference：
Article; Mohamed, Tarek; Yeung, Jacky C.K.; Rao, Praveen P.N.; Bioorganic and Medicinal Chemistry Letters; vol. 21; 19; (2011); p. 5881 – 5887;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.21655-48-1,cis-2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

A vial was charged with 5-amino-3,6-dichloro-l ,2,4-triazine (495.1 mg, 4.25 mmol) and triethylamine (1.5 mL, 10.76 mmol), 2,6-dimethylpiperazine (0.7054 g, 4.28 mmol) in dioxane (11 mL). The mixture was heated at 95 C for 1.5 h using microwave. The mixture was cooled to room temperature, filtered and the white solid was washed with dichloromethane. The organic solution was concentrated. The residue was dissolved in dichloromethane, washed with saturated potassium carbonate, dried over anhydrous sodium sulfate, concentrated. The residue was purified with flash column chromatography on silica gel using ethyl acetate and 0-10% methanol/ethyl acetate to afford product as solid (0.8916 g, yield: 86%). NMR (500 MHz, Chloroform-i/) delta 5.168 (br, 2H), 4.550 (d, J = 12.5 Hz, 2H), 2.859-2.800 (m, 2H), 2.432 (d, – J= 13.2 Hz, 1 H), 2.406 (d, J= 10.5 Hz, 1H), 1.094 (d, J = 6.5 Hz, 6H). LC-MS: 243.0 (MH+/z).

21655-48-1, As the paragraph descriping shows that 21655-48-1 is playing an increasingly important role.

Reference：
Patent; NEKTAR THERAPEUTICS (INDIA) PVT. LTD.; NEKTAR THERAPEUTICS; SHARMA, PANKAJ; KHATRI, VIJAY KUMAR; GU, XUYUAN; SONG, YUAN; SHEN, MICHAEL LIXIN; SAUTHIER, JENNIFER RIGGS; ANAND, NEEL K.; KOZLOWSKI, ANTONI; ODINECS, ALEKSANDRS; RILEY, TIMOTHY A.; REN, ZHONGXU; MU. YONGQI; SHEN, XIAOMING; YUAN. XUEJUN; AURRECOECHEA, NATALIA; O’MAHONY, DONOGH JOHN ROGER; WO2015/92819; (2015); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109384-27-2,1-Methylpiperazin-2-one hydrochloride,as a common compound, the synthetic route is as follows.

A solution of 5-chloro-3-(1-methyl-1H-pyrazol-4-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[4,3-d]pyrimidine (40 mg, 0.110 mmol), 1-methylpiperazin-2-one hydrochloride (33.0 mg, 0.219 mmol), and N,N-diisopropylethylamine (56.7 mg, 0.438 mmol) in dioxane (1 mL) was heated to 100 C. After 20 hrs, the reaction was cooled to r.t., diluted with water and extracted with EtOAc. The organic layer was washed with brine, dried with Na2SO4 and concentrated. The crude was taken up in 1 mL MeOH and 1 mL HCl (4 M solution in dioxane) and stirred at 60 C. for 2 hrs. The resulting mixture was purified with prep-LCMS (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.1% TFA, at flow rate of 60 mL/min). LCMS calculated for C14H17N8O (M+H)+: m/z=313.1; found 313.1. The product was isolated as the TFA salt., 109384-27-2

As the paragraph descriping shows that 109384-27-2 is playing an increasingly important role.

Reference：
Patent; Incyte Corporation; Vechorkin, Oleg; Nguyen, Minh; Qi, Chao; Wang, Anlai; Wu, Liangxing; Yao, Wenqing; Zhao, Peng; (82 pag.)US2020/95250; (2020); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

74879-18-8,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.74879-18-8,(S)-(+)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

c) A mixture of (R)-6-bromo-l-(l-(4-chloro-2-(trifluoromethyl)phenyl)ethyl)-lH- benzo[i/]imidazole (0.25 g, 0.62 mmol), (5)-(+)-2-methylpiperazine (0.13 g, 1.3 mmol), Pd2(dba)3 (0.028 g, 0.031 mmol), BetaGammaNuAlphaRho (0.057 g, 0.093 mmol), and Cs2C03 (0.60 g, 1.9 mmol) in toluene (10 mL) was purged with nitrogen for 5 min, and then heated at 100 C for 16 h. After cooling to room temperature, the mixture was filtered and washed with EtOAc (10 mL). The filtrate was concentrated in vacuo. The resulting crude mixture was diluted with ethyl acetate (20 mL), washed with deionized water and brine, dried ( a2S04), and concentrated in vacuo. The resulting crude material was purified by flash chromatography (Si02, 0-20% methanol in dichloromethane) to afford the coupled product (0.13 g, 0.24 mmol, 39%).

As the paragraph descriping shows that 74879-18-8 is playing an increasingly important role.

Reference：
Patent; CHEMOCENTRYX, INC.; LELETI, Manmohan Reddy; LI, Yandong; MALI, Venkat Reddy; POWERS, Jay; YANG, Ju; WO2013/82429; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.129799-15-1,Methyl 1-Boc-piperazine-2-carboxylate,as a common compound, the synthetic route is as follows.

Step 6 Synthesis of 4-(5-Fluoro-2-trifluoromethyl-benzoyl)-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester DIPEA (430 mg, 0.58 mL, 3.27 mmol) followed by HOBT (121 mg, 0.9 mmol) and EDCI (230 mg, 1.22 mmol) were added to a stirred solution of 5-Fluoro-2-trifluoromethyl-benzoic acid (170 mg, 0.82 mmol) in DMF (2.0 mL) at room temperature. After 2 minutes 2 minutes piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (200 mg, 0.82 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added, filtered the solid precipitated to afford 305 mg (85.9%) of 4-(5-Fluoro-2-trifluoromethyl-benzoyl)-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester.

129799-15-1, As the paragraph descriping shows that 129799-15-1 is playing an increasingly important role.

Reference：
Patent; Bischoff, Alexander; Subramanya, Hosahalli; Sundaresan, Kumar; Sammeta, Srinivasa Raju; Vaka, Anil Kumar; US2010/160323; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

70261-81-3, 1-Methyl-4-(4-nitrobenzyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

70261-81-3, 8.5 g (36.2 mmol) of crude I-a, 2.0 g of FeO(OH)/C catalyst and 100 mL of 95% ethanol were added to a 500 mL one-necked flask, and the mixture was heated under reflux, and a mixture of 25 mL of hydrazine hydrate and 20 mL of 95% ethanol was slowly added dropwise. The disappearance of the starting material by TLC (methanol: chloroform = 1:15). The filter cake was washed twice with hot ethanol (30 mL × 2). The solvent was evaporated under reduced pressure to give a white solid. Vacuum drying (I-a’) 6.7 g, The yield was 90.3%. The product was directly fed to the next reaction without further purification.

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Shanghai Fuxing Pharmaceutical Industrial Co., Ltd.; Lu Shuai; Jin Qiaomei; Wang Yue; Chen Yadong; Lu Tao; (54 pag.)CN104592251; (2019); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a stirred suspension of 1-fluoro-4-nitrobenzene (2 g,14.17 mmol) and potassium carbonate (3.92 g, 28.3 mmol) in anhydrous dimethyl sulfoxide (10 mL) was added 2- (piperazin-1-yl)ethanol (2.089 mL, 17.01 mmol) and the mixture was heated at 80 C for 16 hours. After coolingthe mixture was partitioned between water (100 mL) and ethyl acetate (30 mL) . The aqueous layer was separated and extracted with ethyl acetate (2 x 30 mL) . The combined organic fractions were reduced in vacuo. The residue was triturated in water (100 mL) . The solid wascollected by filtration under vacuum and dried for 16 hours under vacuum and flowing nitrogen to give the title compound (3.45 g, 97 %) . ?H NMR (400 MHz, CDC13) : 3 8.11 (d, 2H), 6.82 (d, 2H), 3.68 (t, 2H), 3.44 (t, 4H), 2.67 (t, 4H), 2.62 (t, 2H), 2.55 (br s, 1H) . LCMS (Method C):RT = 0.45 mi m/z = 252 [M+H]., 103-76-4

103-76-4 N-(2-Hydroxyethyl)piperazine 7677, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ALMAC DISCOVERY LIMITED; HARRISON, Timothy; TREVITT, Graham; HEWITT, Peter Robin; O’DOWD, Colin Roderick; BURKAMP, Frank; WILKINSON, Andrew John; SHEPHERD, Steven D.; MIEL, Hugues; WO2015/92431; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.13754-38-6,1-Benzoylpiperazine,as a common compound, the synthetic route is as follows.

13754-38-6, General procedure: A solution of 2-chloroalkyl/aryl substitutedwith or without N-substitution as well as with or without 5 and/or 6-substituted benzimidazole derivative (1.75g,0.01051mol) and 1-[(4-phenyl)carbonyl]piperazine (3g,0.0105mol) in N, N dimethylformamide was taken in a RBF.K2CO3(2gm,) was added to the reaction mixture. The reaction mixture was stirred for 8h at 80C on a magnetic stirrer (heat + stirring). The progress of the reaction was monitored by thin layer chromatography (TLC).Upon completion of the reaction, water was added to the reaction mixture and the product extracted by shaking the reaction mixture with dichloromethane in a separating funnel.The dichloromethane layer was washed successively with water and brine, dried over anhydrous sodium sulfate. Evaporation of the solvent gave theproduct. 11a-l Recrystallized with various solvent like chloroform, ethanol, methanol.(4-((1H-benzo[d]imidazol-2-yl) methyl) piperazin-1-yl)(Phenyl) methanone (11a) Compound 11a was obtained as a white solid (yield: 74.35%; MP:224-226; IR (KBr): 3220(N-H), 2365 (C-H), 1670(C=O),1604(C=N),1556(C=C), 1232 (C-N) cm-1; 1H NMR (300 MHz,CDCl3)ppm: 3.45-3.51(m, 4H,PIP-H), 4.34(s, 2H,-CH2-), 4.79(s, 1H, N-H), 7.30-7.45 (m, 4H, Ar -H of Benzim) 7.89-8.07 (4H, Ar -H of benzoyl) ; 13C-NMR(400 MHz, CDCl3, TMS): 52.14 (CH2), 55.4(CH2),61.7 (CH2), 117(arom. CH), 124 (arom. CH),129(arom. CH), 133.5 (quat. C), 139.8 (quat. C), 145.6(quat. C),171.6 (carbonyl C).ESI-MS m/z:320,243,189,131.Anal. Calcd. for C19H20N4O(320): C, 71.23; H, 6.29; N, 17.49; O, 4.99. Found: C,71.10; H, 6.23; N, 17.43; O, 4.91

The synthetic route of 13754-38-6 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Kankate, Rani S.; Gide, Parag S.; Belsare, Deepak P.; Oriental Journal of Chemistry; vol. 30; 4; (2014); p. 1855 – 1863;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109384-27-2,1-Methylpiperazin-2-one hydrochloride,as a common compound, the synthetic route is as follows.,109384-27-2

EXAMPLE 21b (4-methyl-3-oxopiperazin-1-yl)acetic acid The compound can be prepared in the following way: A solution of 0.61 g of 2-bromoacetic acid, 10 ml of water, 0.74 g of 1-methyl-piperazin-2-one hydrochloride (commercially available product) and 0.61 g of potassium carbonate is kept stirred at a temperature in the vicinity of 20 C. for 18 hours. 0.31 g of potassium carbonate is then added and stirring is maintained for one hour. The reaction medium is acidified (pH~1) by addition of an aqueous hydrochloric acid solution (1N) and then concentrated by evaporation under reduced pressure. The residue obtained is taken up in 2 times 30 ml of toluene and then concentrated. The yellow solid obtained is taken up in 5 ml of ethanol, filtered off on a sintered glass funnel and washed with 2 times 5 ml of ethanol. The filtrate is concentrated by evaporation under reduced pressure and 1.03 g of (4-methyl-3-oxopiperazin-1-yl)acetic acid hydrochloride are thus obtained in the form of a yellow foam. MS: method A; [M+H]+: m/z=173; [M-H]-: m/z=171; Tr=0.11 min.

The synthetic route of 109384-27-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; sanofi-aventis; US2011/263593; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics