Month: September 2021

1228780-72-0, 1-((4′-Chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2-yl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

In a 500-mL three necked round bottom flask equipped with magnetic stirrer, thermometer, condenser, charged 4-bromo-2-(1H-pyrrolo[2,3-b]pyridine-5-yloxy)benzoic acid (8.67 g, 26 mmol), (4-(N,N-dimethylamino)phenyl)-di-tert-butyl-phosphine (APhos, 895 mg, 0.78 mmol, 0.13 equiv), tris(dibenzylideneacetone)-dipalladium(0) (1.54 g, 1.69 mmol, 0.065 equiv), THF (87 mL) and 1-[[2-(4-chlorophenyl)-4,4-dimethylcyclohex-1-enyl]methyl]piperazine in toluene (31.2 g, 29 mmol, 1. 12 equiv). The reaction mixture was stirred under inert atmosphere, 1.5 M lithium bis(trimethylsilyl)amide in THF (74 mL, 112 mmol, 4.3 equiv) was added, and heated to 55-56C. The reaction mixture was stirred at 55-56C for 30 min then quenched by addition of cold (2-8C) 12% aqueous NaCl (347 mL). After phase separation the organic layer was filtered and concentrated in vacuum to 1/3 volume. The residue was added to a cold (0-5C) suspension of perlite (22 g) in n-heptane (364 mL). The suspension was stirred for 1 hour at 0-5C then filtered. The wet-cake was washed with n-heptane (3 x87 mL), and dried under vacuum at 20-25C for 2 hours. The solid was suspended in THF (87 mL), filtered and the wet cake was washed with THF (4×87 mL). HPLC-analysis of the combined THF solution comprised 8.3 g of VNT-08 content (yield: 56%).

1228780-72-0, 1228780-72-0 1-((4′-Chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2-yl)methyl)piperazine 66713599, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ASSIA CHEMICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; POTARINE JUHASZ, Zsuzsa; STRUBA, Szabolcs; NEMETHNE RACZ, Csilla; TOTH, Zoltan Gabor; SZILAGYI, Andrea; KERTI-FERENCZI, Renata; MOLNAR, Sandor Janos; PASZTOR-DEBRECZENI, Nora; HAJKO, Janos; (100 pag.)WO2017/156398; (2017); 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.1235865-77-6,2-((1H-Pyrrolo[2,3-b]pyridin-5-yl)oxy)-4-(4-((4′-chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2-yl)methyl)piperazin-1-yl)benzoic acid,as a common compound, the synthetic route is as follows.

4-fluoro-3-nitrobenzenesulfonamide (235 mg, 1.06 mmol, 1.00 eq) and2 – ((1H-pyrrolo [2,3-b] pyridin-5-yl) oxy) -4- (4 – ((4′-chloro-5,5-dimethyl- , 6-tetrahydro- [1,1′-biphenyl] -2-yl) methyl) piperazin-1-yl) benzoic acid(600 mg, 1.06 mmol, 1.0 eq) (see Example 1, Step 14) was added to 6 mL of phosphorus oxychloride and reacted at 85 C for 5 h. The reaction solution was poured into 20 mL of ice water and extracted with EA (10 mL x 3). The organic phase was separated, dried over anhydrous sodium sulfate, dried over the column, PE / EA (v / v) = 2/1 and DCM / EtOH (v / v) = 10/1 as an eluent to give 830 mg of a white solid product in 100% yield.

1235865-77-6, As the paragraph descriping shows that 1235865-77-6 is playing an increasingly important role.

Reference：
Patent; Sunshine Lake Pharma Co.,Ltd.; Kou, Yuhui; Hu, Bolin; Jiang, Haigang; Ye, Jiuyong; Liu, Zhiqiang; Xie, Hongming; Zhang, Yingjun; (42 pag.)CN106565706; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5308-25-8,5308-25-8, 1-Ethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A solution of compound 2 (0.55 mmol), 1-substituted piperazine (0.83 mmol) and pyridine (0.8 mmol) in 10 mL THF (tetrahydrofuran) was stirred at room temperature overnight. When the reaction was completed, the solvent was evaporated under reduced pressure. The residues were dissolved in ethyl acetate and washed with water and saturated sodium chloride solution. After drying over anhydrous Na2SO4, the solvent was removed under reduced pressure to get crude product. The pure products were obtained by recrystallizing from ethanol.

The synthetic route of 5308-25-8 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Wu, Zhilin; Ding, Na; Tang, Yuting; Ye, Jiao; Peng, Junmei; Hu, Aixi; Research on Chemical Intermediates; vol. 43; 8; (2017); p. 4833 – 4850;,
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.1589082-06-3,(S)-tert-Butyl 3-(cyanomethyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

A reaction mixture of tert-butyl (3S)-3-(cyanomethyl)piperazine-1-carboxylate (850 mg, 3.77 mmol) and HCl/dioxane (4 M, 20 mL) was stirred at 15° C. for 1 hour. Upon completion, the solvent was removed under vacuum to give 2-[(2S)-piperazin-2-yl]acetonitrile (740 mg, 3.74 mmol, 99.0% yield, 2HCl) as a white solid. 1H NMR (400 MHz, METHANOL-d 4) delta=4.04-3.90 (m, 1H), 3.81-3.70 (m, 2H), 3.69-3.61 (m, 2H), 3.53-3.36 (m, 2H), 3.13 (d, J=6.4 Hz, 2H)., 1589082-06-3

The synthetic route of 1589082-06-3 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

4318-42-7,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4318-42-7,1-Isopropylpiperazine,as a common compound, the synthetic route is as follows.

In N2 Under protection, three-necked flask with stirring and the funnel was added dropwise and THF150ml 100mmol isopropyl piperazine, in an ice bath, was slowly added dropwise through a dropping funnel 100mmol butyllithium dropwise after l to room temperature, the reaction after 1h.Under a 71/92 then cooled to 0°C 100mmol cyclohexyl trimethoxysilane, after the completion of the dropwise addition the reaction at room temperature for 8h, and finally through G4Funnel, the solid residue was washed repeatedly with tetrahydrofuran and filtered, the filtrate was collected.With a rotary evaporator to tetrahydrofuran solvent, vacuum distillation, collecting 136 ~ 139°C / 100pa fraction.Vacuum distillation, collecting 136 ~ 139°C/ 100pa distillate, heavy 5.3g, 98.2percent yield,

As the paragraph descriping shows that 4318-42-7 is playing an increasingly important role.

Reference：
Patent; Institute of Chemistry Chinese Academy of Sciences; Li, Huayi; Chang, Hefei; Zhang, Liaoyun; Hu, Youliang; (19 pag.)CN102977133; (2016); B;,
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.4318-42-7,1-Isopropylpiperazine,as a common compound, the synthetic route is as follows.

General procedure: To a solution of compound 9 (100mg, 0.23mmol) in CH2Cl2 (10ml) was added oxalyl chloride (0.04ml, 0.50mmol) at 0°C, the reaction mixture was stirred at 0°C for 0.5h and then at room temperature for another 3h. The mixture was added to a solution of various amines (2.2 eq) and Et3N (0.1ml, 0.72mmol) and stirred for 12hat room temperature. After the reaction completed, the mixture was washed by water (3×20ml), brine (2×20ml), dried over anhydrous Na2SO4 and concentrated, the residue was purified by silica gel chromatography (CH2Cl2/MeOH 30/1v/v) to give corresponding diamides 10?26.

4318-42-7, 4318-42-7 1-Isopropylpiperazine 78013, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Mao, Shi-Wei; Chen, Huang; Yu, Li-Fang; Lv, Fang; Xing, Ya-Jing; Liu, Ting; Xie, Jia; Tang, Jie; Yi, Zhengfang; Yang, Fan; European Journal of Medicinal Chemistry; vol. 122; (2016); p. 574 – 583;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

630125-91-6, 4-((4-Ethylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 3-(2-(cyclopropanecarboxamido)thiazolo[5,4-b]pyridin-5-yl) benzoic acid (150 mg, 0.44 mmol) and triethylamine (90 muL, 0.66 mmol) in toluene (2 niL) was added diphenylphosphoryl azide (0.11 niL, 0.49 mmol). The resulting mixture was stirred at room temperature for 30 minutes and heated at 80 0C for 1 h. To a reaction mixture was added 4-((4-ethylpiperazin-l-yl)methyl)-3-(trifluoromethyl) aniline (121 mg, 0.42 mmol) and triethylamine (90 muL, 0.66 mmol). The reaction mixture was stirred at 80 0C for 2h and most of organic solvent was removed in vacuo. The crude product was diluted with DMSO (3 mL) and purified by preparative HPLC to give the title compound as a TFA salt.1H NMR 600 MHz (CDCl3) delta 8.51 (s, IH), 7.83 (d, J= 1.8 Hz, IH), 7.48 (m, 2H), 7.19 (m, 3H), 7.12 (m, 2H), 6.85 (J, J= 3.0 Hz, IH), 6.49 (m, IH), 6.19 (m, 2H), 3.84 (m, IH), 3.78 (s, 3H), 3.46 (m, 2H), 3.19 (m, IH), 2.90 (m, 2H), 1.99 (m, 2H), 1.69 (m, 2H), 1.19 (J, J= 6.6 Hz, 6H), MS m/z : 624.36 (M + 1).

630125-91-6, 630125-91-6 4-((4-Ethylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline 59134564, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; NOVARTIS AG; CHOI, Hwan, Geun; SIM, Taebo; GRAY, Nathanael; ZHOU, Wenjun; CHANG, Jae, Won; ZHANG, Jianming; WEISBERG, Ellen; WO2010/144909; (2010); A1;,
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

131.5 g of N-hydroxyethylpiperazine (purity 99%, about 1 mol)And 30% (mass concentration) aqueous sodium vinyl sulfonate solution (containing 1.05 mol of sodium vinyl sulfonate)Was added to a 1000 mL four-necked flask equipped with a reflux tube,The addition reaction is carried out with sufficient stirring;The reaction was carried out at 60 C for 1.0 hour,And then gradually heated to boiling reflux (about 100 ~ 120 , depending on the composition of the reaction and change)And continue to react for 2.0 hours;then,Cooled to give a reaction mother liquorcontaining 4-hydroxyethylpiperazineethanesulfonate.By high performance liquid chromatography,The yield of sodium 4-hydroxyethylpiperazineethanesulfonate was calculated to be 95.2%.A reaction mother liquor containing 0.5 mol HEPES-Na at a mass concentration of 40 wt% was placed in a 500 mL beaker,Under stirring,At room temperature,27.3 g of oxalic acid (99 wt%) was added slowly,Then stir,And acidified at 20 C for 1 hour.Into the low temperature thermostat,Cooling to 10 ,Cooling crystallization for 0.5 hours,The precipitated sodium oxalate was removed by filtration.The filtrate was placed in a beaker,Constantly stirring,1.0 g of Ba (OH) 2 was slowly added,Reaction for 1 hour,Remove the sulfate.Adding 5 g of activated carbon decolorization and filtering by filtration to obtain the filtrate,By rotary evaporation to anhydrous,To obtain a solid primary purified product.The solids were washed three times with 500 ml of ethanol,And then vacuum drying,Get high purity HEPES.

103-76-4, As the paragraph descriping shows that 103-76-4 is playing an increasingly important role.

Reference：
Patent; Shandong University of Technology; Cui Hongyou; Wang Jiangang; Zhu Liwei; Liu Ransheng; Yang Yong; Wang Yang; (8 pag.)CN104803949; (2017); B;,
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.78551-60-7,tert-Butyl 4-benzyl-3-oxopiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

78551-60-7, To a solution of the product of Step 8 (261 mg, 0.900 mmol) in anhydrous THF(5 ml) in a dry ice-acetone bath was added 2M LDA (0.45 ml) and the mixture wasstirred for 1 h. A solution of the above aldehyde in THF (5 ml) was added and themixture was stirred in the dry ice-acetone bath for 2 h. The reaction was quenchedwith saturated NH4CI (4 ml), diluted with CH2CI2 (50 ml), and washed with water (30ml). The organic layer was extracted with saturated NH4CI and brine, dried (MgSO4),concentrated, and purified by PTLC (5% MeOH/CH2CI2) to give the product (100 mg,48%). MS m/e 699 (M+H)+

78551-60-7 tert-Butyl 4-benzyl-3-oxopiperazine-1-carboxylate 10891590, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; SCHERING CORPORATION; WO2006/14944; (2006); 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.21655-48-1,cis-2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

General procedure: A solution of intermediate4a or 4b (1mmol), corresponding aliphatic amine (2mmol), K2CO3 (2mmol) in DMF was stirred at room temperature overnight. DMF was removed in vacuo and then H2O was added. The layer was extracted with CH2Cl2 (15mL×3). Organic layers were dried on Na2SO4 and the solvent was removed under pressure. Compounds were purified by column chromatography using dichloromethane/methanol as an eluent to give 5a-11a and 12b-21b.

21655-48-1, 21655-48-1 cis-2,6-Dimethylpiperazine 6950261, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Wang, Yu; Chen, Shaowei; Hu, Gang; Wang, Jiao; Gou, Wenfeng; Zuo, Daiying; Gu, Yucheng; Gong, Ping; Zhai, Xin; European Journal of Medicinal Chemistry; vol. 143; (2018); p. 123 – 136;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics