Month: May 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.129799-08-2,1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate,as a common compound, the synthetic route is as follows.

Step 1: To a solution of piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (10.6 g, 43 mmol) in 250 mL of dichloromethane was added (Boc)2O (19 g, 86 mmol) at 0 C. The reaction mixture stirred for 4 hours at room temperature, and then quenched with water and then extracted with dichloromethane. After the organic layer was dried over anhydrous Na2SO4, the filtrate was concentrated. The residue was purified by silica gel column chromatography to give Compound AH (yield 13.6 g, 92%)., 129799-08-2

129799-08-2 1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate 2756819, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; HOFFMANN-LA ROCHE INC.; Guo, Lei; Hu, Taishan; Kou, Buyu; Lin, Xianfeng; Shen, Hong; Shi, Houguang; Yan, Shixiang; Zhang, Weixing; Zhang, Zhisen; Zhou, Mingwei; Zhu, Wei; US2015/252057; (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.30459-17-7,1-(4-Trifluoromethylphenyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: Arylpiperazines (1.2 equiv) and potassium carbonate (4.0equiv) were added to a solution of 1 (1 equiv) in acetonitrile(CH3CN, 20 mL). The reaction mixture was heated to 85 Cand stirred for 12 h. Afterward the mixture was cooled toroom temperature. The reaction mixture was filtered, and thefiltrate was concentrated in vacuo. The residue was extractedwith ethyl acetate (60 mL) and water (20 mL). After dryingthe organic layer with anhydrous Na2SO4and evaporatingthe solvent under reduced pressure, a solid was appeared.The solid was recyrstallized from ethanol to obtain intermediates2.

30459-17-7, As the paragraph descriping shows that 30459-17-7 is playing an increasingly important role.

Reference：
Article; Chen, Hong; Jia, Huixia; Qian, Yuna; Shen, Jianliang; Yu, Yuzhong; Zhang, Haibo; Zhao, Shanchao; Pharmacological Reports; (2020);,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59878-57-8, 1-(Cyclopropylcarbonyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,59878-57-8

1- (3-carboxybenzyl) thieno [2,3-D] pyrimidine-2,4 (1H, 3H) -dione (0.2 g, 0.66 mmol) Tripyrrolidinium bromide phosphonium hexafluorophosphate (PyBrOP, 0.46 g, 0.99 mmol), 1-cyclopropanecarbonylpiperazine (0.1 g, 0.66 mmol), N, N-diisopropylethylamine (DIPEA, 0.17 g, 1.32 mmol), dichloromethane (5 mL) was added to the reaction flask, Stir overnight at room temperature. The reaction mixture was added with methylene chloride (5 mL), water (5 mL), extracted, The organic layer was washed with water (3 mL), dried, filtered and concentrated to give the crude product. The crude product was purified by silica gel column chromatography (mobile phase CH2Cl2 / CH3OH 50/1) to give the final product Synthesis of 1- (3- (4-cyclopropylcarbonylpiperazine-1-carbonyl) benzyl) thieno [2,3- D] pyrimidine-2,4 (1H, 3H) Dione (I-1) as a white solid (0.2 g, yield 68.9%),

59878-57-8 1-(Cyclopropylcarbonyl)piperazine 2064235, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Shanghai Xunhe Pharmaceutical Technology Co., Ltd.; Zheng Yongyong; Jin Hua; Zhou Feng; Huang Meihua; Meng Xin; (28 pag.)CN107286174; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

31166-44-6, 1-Cbz-Piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of tert-butyl 2,4-dichloro-8-oxo-5,8-dihydropyrido[3,4-d]pyrimidine-7(6H)-carboxylate (0.400 g, 1.26 mmol) in CH 2Cl 2 (5.0 mL) was added N,N-Diisopropylethylamine (0.325 g, 2.51 mmol) followed by benzyl 1-piperazinecarboxylate (0.255 mL, 1.32 mmol) and the reaction stirred at ambient temperature for 1.5 h. The reaction mixture was diluted with CH 2Cl 2 (10 mL) and washed with a 0.5M KHSO 4 solution (5 mL), followed by a saturated aqueous NaHCO 3 solution and brine. The organic layer was dried over Na 2SO 4, filtered and concentrated. The crude product was sonicated in 10 mL MTBE and the resulting solid was isolated by vacuum filtration. The solid was dried in vacuo to provide 0.507 g (80%) of the desired product as an off-white solid which was used directly in the next step. ES+APCI MS m/z 502.1[M+H] +.

31166-44-6, The synthetic route of 31166-44-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Mirati Therapeutics, Inc.; Array BioPharma Inc.; Blake, James F.; Burgess, Laurence E.; Chicarelli, Mark Joseph; Christensen, James Gail; Cook, Adam; Fell, Jay Bradford; Fischer, John P.; Marx, Matthew Arnold; Mejia, Macedonio J.; Savechenkov, Pavel; Vigers, Guy P.A.; Smith, Christopher Ronald; Rodriguez, Martha E.; US2019/144444; (2019); 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.325145-35-5,(S)-tert-Butyl 2-ethylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

ER-895473 (103 mg, 0.261 mmol, 27.1percent yield) was prepared in a similar manner to ER-899742 starting with 38 (286 mg, 0.962 mmol) and (S)-tert-butyl 2-ethylpiperazine-1-carboxylate (206 mg, 0.962 mmol). DMF (3 mL) was used instead of DCM for the amide forming reaction and 2.0 M HCl in ethyl ether (1.3 mL, 2.6 mmol) was used in the Boc-deprotection process using acetonitrile (1 mL) as a solvent. ER-895473 was purified by reverse-phase HPLC (X-Bridge C18 19×100 mm column; eluting with a gradient of increasing acetonitrile in water containing 0.1percent formic acid). The product fractions were combined and concentrated to dry followed by dilution in MeOH (1 mL), passed through as basic silica gel plug (Biotage SiCO3, 1 g, eluting with MeOH (1 mL)), concentrated and dried in vacuo.To a stirred solution of 38 (300 mg, 1.01 mmol) in DCM (2 mL) was added the mixture of (3S,4R)-tert-butyl 3-amino-4-fluoropyrrolidine-1-carboxylate and (3R,4S)-tert-butyl 3-amino-4-fluoropyrrolidine-1-carboxylate, 77 (205.3 mg, 1.005 mmol), HBTU (247 mg, 1.211 mmol) and DIEA (0.70 mL, 4.04 mmol) followed by stifling at rt for 16 h. The was found complete and concentrated to dryness followed by dissolving in EtOAc (20 mL), washed 1 time with water (10 mL), 2 N citric acid in water (10 mL), saturated NaHCO3 (10 mL), and brine (10 mL). The combined aqueous layers were extracted 3 times with EtOAc (10 mL ea.) after which time the combined organic fractions were dried over MgSO4, filtered and concentrated to dry. The crude product was purified over a 25 g Biotage silica gel column eluting with 0-10percent MeOH in DCM (200 mL total) to provide the diastereomeric mixture of 78 and 79., 325145-35-5

Big data shows that 325145-35-5 is playing an increasingly important role.

Reference：
Patent; CARLSON, ERIC; HANSEN, HANS; HAWKINS, LYNN; ISHIZAKA, SALLY; MACKEY, MATTHEW; SCHILLER, SHAWN; OGAWA, CHIKAKO; DAVIS, HEATHER; US2015/105370; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

169447-70-5, (S)-tert-Butyl 2-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a rt solution of 7-bromo-l-((2-(trimethylsilyl)ethoxy)methyl)-lH-indole (3.8 g, 11.64 mmol) in anhydrous toluene (100 mL) was added (S)-tert-butyl-2-methylpiperazine-l- carboxylate (2.79 g, 13.98 mmol), Pd2(dba)3 (1.07 g, 1.17 mmol), t-BuONa (2.24 g, 23.29 mmol), and BINAP (1.45 g, 2.33 mmol) under nitrogen. The reaction mixture was stirred at 80C for 3 hrs, then cooled to rt, diluted with H20 (200 mL), and extracted with EtOAc (100 mL x 2). The combined organic layers were washed with brine (100 mL), dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by chromatography (silica, EtOAc/PE = 1/10) to afford (S)-tert-butyl-2-methyl-4-(l-((2-(trimethylsilyl)ethoxy)methyl)-lH-indol-7- yl)piperazine-l-carboxylate (2.6 g, 5.83 mmol, 50.1%) as a yellow oil. ESI-MS (EI+, m/z): 446.3 [M+H]+., 169447-70-5

As the paragraph descriping shows that 169447-70-5 is playing an increasingly important role.

Reference：
Patent; NAVITOR PHARMACEUTICALS, INC.; O’NEILL, David John; SAIAH, Eddine; KANG, Seong Woo Anthony; BREARLEY, Andrew; BENTLEY, Jonathan; (184 pag.)WO2018/89493; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

57260-71-6, tert-Butyl piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,57260-71-6

S1: N-Boc-piperazine (1.82 kg, 9.77 mol) was added to a 20 L four-necked flask with mechanical stirring and a thermometer.Triethylamine (1.48 kg, 14.66 mol), dichloromethane 5.46 Kg, cooled to 0 C,Cyclopropylcarbonyl chloride (1.12 kg, 10.75 mol) was slowly added dropwise, and the temperature was controlled from 0 C to 10 C.After the completion of the dropwise addition, the reaction was carried out for 3 hours at 10 C to 20 C.Add 5kg of water, add sodium carbonate to adjust pH=8-9, separate the liquid, collect the organic phase, add 1.50Kg of water phase, and extract once with dichloromethane.The methylene chloride phases were combined, washed once with 2 kg of 0.05 M diluted hydrochloric acid, and once with 2 kg of water.The dichloromethane was concentrated to remove 2.43 kg of 4-(cyclopropanecarbonyl)piperazine-1-carboxylic acid tert-butyl ester, yield 98%.The nuclear magnetic warp alignment is consistent with the standard map.

57260-71-6 tert-Butyl piperazine-1-carboxylate 143452, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Suzhou Laikeshide Pharmaceutical Co., Ltd.; Liu Tongchang; Yu Jurong; (6 pag.)CN108341792; (2018); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

325145-35-5, (S)-tert-Butyl 2-ethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A mixture of 2-carboxyl-1H-benzo[d]immidazole-4-carboxamide (75 mg, 0.37 mmol), EDC (210 mg, 1.09 mmol), HOBt(147 mg, 1.09 mmol), Et3N (0.4 mL, 2.93 mmol) and N-Boc-aminopyrrolidine(202 mg, 1.09 mmol) in DMF (5 mL) was stirred atroom temperature for 20 h and then H2O was added to the mixture.The solutionwas extracted with the solvent mixture (ethyl acetate/methanol = 10:1) (30 mL x 3) and then the organic layer waswashed with brine (20 mL x 2). The combined organic layer wasdried over anhydrous MgSO4. After filtration and concentration, thecrude product was obtained and purified with column chromatography(methylene chloride/methanol 50:1 to 40:1) to givecompound 7a as a white solid (74 mg, 54.4percent).

325145-35-5, The synthetic route of 325145-35-5 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Zhou, Jie; Ji, Ming; Zhu, Zhixiang; Cao, Ran; Chen, Xiaoguang; Xu, Bailing; European Journal of Medicinal Chemistry; vol. 132; (2017); p. 26 – 41;,
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.

Example 6 To a solution of Compound A (0.3 g, 0.73 mmol) in acetonitrile (6 mL) at room temperature were added diisopropylethylamine (0.5 mL, 2.9 mmol) and cis-2,6-dimethylpiperazine (0.125 g, 1.09 mmol) and the reaction mixture was heated to 80° C. On heating, the reaction mixture became clear and after 15 min commencement of precipitation of solid was observed. Heating was continued for 3 hr and then the reaction mixture was cooled. The solid obtained was collected by filtration, washed with acetonitrile and dried under vacuum. LC/MS: (M+H)+: 489. An NMR spectrum is provided in FIG. 6.Yield: 0.26 g (73percent)., 21655-48-1

The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Sudhakar, Anantha; US2011/105497; (2011); 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.208167-83-3,tert-Butyl 4-(2-chloroethyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

General procedure: A mixture of compound 9 (200mg, 0.8mmol), sodium iodine (289mg, 1.93mmol) and substituted amines (1.61mmol) in methanol (30mL) was stirred at 40C for 5h. After the reaction was completed (monitored by TLC), the solution was concentrated under vacuum. Then the crude residue was purified by column chromatography (dichloromethane/methanol), affording pure product 10.

208167-83-3, As the paragraph descriping shows that 208167-83-3 is playing an increasingly important role.

Reference：
Article; Liang, Yu-Kun; Yue, Zhi-Zhou; Li, Jia-Xin; Tan, Cun; Miao, Ze-Hong; Tan, Wen-Fu; Yang, Chun-Hao; European Journal of Medicinal Chemistry; vol. 84; (2014); p. 505 – 515;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics