Month: July 2021

13754-38-6, 1-Benzoylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,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.

As the paragraph descriping shows that 13754-38-6 is playing an increasingly important role.

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.304897-49-2,tert-Butyl 4-(4-aminobenzyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Step 1. Preparation of tert-Butyl 4-(4-(4-bromobenzamido)benzyl)piperazine-1-carboxylate (3) 4-Bromobenzoic acid (1, 685.0 mg, 3.4 mmol) and HATU (1298.1 mg, 3.4 mmol) are partially dissolved in DMF (10 mL) at rt. DIEA (560 muL, 3.4 mmol) is added to this mixture to give a pale yellow solution. After stirring at rt for 30 min, tert-butyl 4-(4-aminobenzyl)piperazine-1-carboxylate (2, 992.9 mg, 3.4 mmol) is added and the resulting reaction mixture is heated at 60 C. for 20 h, allowed to cool to rt, and poured into water (100 mL). This mixture is extracted with Et2O (3*150 mL). The combined organic extracts are evaporated to dryness to give a white solid, which is washed with water (50 mL) and dried in vacuo. This material is used in the next synthetic step without further purification. HPLC: tR 1.67 min (method 1). LC-MS m/z calcd for C23H2879BrN3O3 ([M]+), 473. found, 474 ([M+H]+). 1H NMR (CD3OD): delta 1.46 (s, 9H), 2.96 (m, 4H), 3.59 (m, 4H), 4.05 (br s, 2H), 7.46 (m, 2H), 7.69 (m, 2H), 7.78 (m, 2H), 7.85 (m, 2H).

304897-49-2, The synthetic route of 304897-49-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ACHILLION PHARMACEUTICALS, INC.; Wiles, Jason Allan; Gadhachanda, Venkat; Chen, Dawei; Wang, Qiuping; Hashimoto, Akihiro; Pais, Godwin; Wang, Xiangzhu; Deshpande, Milind; Phadke, Avinash; US9125904; (2015); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

208167-83-3, tert-Butyl 4-(2-chloroethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

[0384] To a solution of l-Boc-4-(2-chloroethyl)piperazine (6.85 g, 27.62 mmol) in methanol (50 ml) was added thiourea (4.12 g, 55.24 mmol). The mixture was heated to reflux for 2 hours. A solution of sodium hydroxide (1.66 g, 41.43 mmol) in water (10 ml) was added, and the mixture was continued to reflux for another hour. Then most solvent was evaporated under reduced pressure. The residue was mixed with ethyl acetate (50 ml) and brine (30 ml) and separated. The ethyl acetate was dried over magnesium sulfate and evaporated under reduced pressure. The residue was dissolved in methanol (20 ml). 4 M hydrochloric acid in dioxane (10 ml) was added. The mixture was stirred at room temperature overnight and most of solvent was evaporated under reduced pressure. The residue was used for the addition reaction without further purification.

208167-83-3, The synthetic route of 208167-83-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; SU, Zhuang; LONG, Zhengyu; YANG, Suizhou; WO2014/145686; (2014); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

74879-18-8, (S)-(+)-2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

74879-18-8, (S)+-2-methylpiperazine (10 g) was dissolved in acetonitrile (140 ml) and cooled to 5-100C whereupon triethylamine (35 ml) was added, followed by drop wise addition of a solution of trityl chloride 27.9 (g) in DCM (80 ml). The reaction was stirred for 1 h at room temperature. The resulting slurry was cooled to approximately 00C then filtered. The filtrate was evaporated in vacuo and the residue was purified by chromatography (silica, 1-4% MeOH/ DCM as eluent) to give the sub-title compound (29 g).

74879-18-8 (S)-(+)-2-Methylpiperazine 2734219, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/56752; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

A mixture of methyl 2-((lH-pyrrolo[2,3-b]pyridin-5-yl)oxy)-4-fluorobenzoate (500.0 g), l-((4′-Chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[l,l’-biphenyl]-2-yl)- methyljpiperazine (1114.0 g) and N,N-diisopropylethylamine (225.8 g) in dimethylsulphoxide (1500 mL) was heated to 90 to 105 degree Celsius for 26h. The reaction mixture was diluted with ethyl acetate (2500 ml) and washed with water (2500 mL). The organic layer was concentrated under vacuum. The residue was taken up in methanol (2500 mL) at 60 to 65 degree Celsius and cooled to 20 to 30 degree Celsius and stirred for 4h, followed by 0 to 5 degree Celsius for 3h. The resulting slurry was filtered and washed with cold methanol (500 mL). The filtered solid was treated with concentrated hydrochloric acid (218.3 g) in methanol (3200 mL) followed by addition of water (1600 mL). The resulting slurry was cooled to 0 to 5 degree Celsius, filtered and washed with a 2:1 mixture of methanol-water and the solid dried under vacuum at 50 to 60 degree Celsius for 16 h to provide methyl 2-((lH-pyrrolo[2,3-b]pyridin-5- yl)oxy)-4-(4-((4′-chloro-5,5-dimethyl-3,4,5,6-tetrahydro[l,l’-biphenyl]-2- l)methyl)piperazin- 1 -yl)-benzoate. HC1. Yield: 74.14% (805g) HPLC Purity: -99.3% 1H NMR data-(DMS 0-d6) : d 0.942 (s, 6H), 1.444 (t, J=6.4 Hz, 2H), 2.014 (s, 2H), 2.366 (t, br, 2H), 2.723 (d, 2H), 3.281 (m, 4H), 3.702 (m, 2H), (m, d, J=12.8 Hz, 8H), 3.542 (s, 2H), 3.659 (s, 3H), 6.385 (dd, J= 1.6, 2.0, 3.2, 3.6Hz, 1H), 6.414-6.420 (d, =2.4Hz, 1H), 6.776 (dd, J=2.4, 9.2Hz, 1H), 7.105 (d, J=8.4Hz, 2H), 7.395( d, J=8.4Hz, 2H), 7.438 (d, J=2.0, 1H), 7.483 (t, J=2.8Hz, 1H), 7.781 (d, J=9.2Hz, 1H), 7.999 (d, J=2.8Hz, 1H), 10.752 (s, br, 1H), 11.666 (s,lH)., 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; FRESENIUS KABI ONCOLOGY LTD.; GUPTA, Chandan Kumar; DHIMAN, Navdeep; SANGHANI, Sunil; SINGH, Govind; LAHIRI, Saswata; CABRI, Walter; GUPTA, Nitin; (0 pag.)WO2020/3272; (2020); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

170911-92-9, tert-Butyl 4-(4-aminophenyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2,4-Dichloro-5-(trifluoromethyl)pyrimidine (2.39 g, 11.0 mmol) was stirred in a 1 :1 t- BuOH:1 ,2-dichloroethane mixture (80 mL) at 0 C and a 1.0 M ZnCI2 solution in diethyl ether (12.6 mL, 12.6 mmol) was added cautiously over 20 minutes and the reaction was left stirring at 0 C for 30 minutes. A solution of tert-butyl 4- (4- aminophenyl)piperazine-1-carboxylate (12) (2.92 g, 10.5 mmol) in 1 : 1 f-BuOH:1 ,2- dichloroethane (40 mL) was added drop-wise over 15 minutes at 0 C followed by a solution of triethyiamine (1.76 mL, 12.6 mmol) in 1 : 1 ?-BuOH: 1 ,2-dichloroethane (40 mL) and the reaction was allowed to warm to room temperature and was stirred for 18 hours. The organic solvents were evaporated in vacuo and the crude yellow oily solid was suspended in water (400 mL), the suspension was sonicated for 30 minutes and the product was collected by filtration, the solid was washed with water (10 x 20 mL) and dried under a high vacuum to give the title compound (13) (4.75 g, 98% yield) as a beige solid; 1H NMR (400 MHz, cfe-DMSO) delta 10.45 (s, 1 H), 8.72 (s, 1 H), 7.50 (d, J = 8.5 Hz, 2H), 6.96 (d, J = 9.0 Hz, 2H), 3.50 – 3.42 (m, 4H), 3.09 – 3.02 (m, 4H), 1.42 (s, 9H). LCMS Method C: rt 6.56 min; m/z 456.2, 458.1 [M-H]’., 170911-92-9

170911-92-9 tert-Butyl 4-(4-aminophenyl)piperazine-1-carboxylate 11011301, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; CANCER THERAPEUTICS CRC PTY LTD; DEVLIN, Mark Graeme; STREET, Ian Philip; TONG, Warwick Bonner; WO2014/27199; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

132710-90-8, 1-Boc-4-(3-hydroxypropyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Triphenylphosphine (2.059 g, 7.85 mmol), fert-butyl 4-(3- hydroxypropyl)piperazine-l-carboxylate ( 1.692 g, 6.93 mmol) and diisopropyl (E)- diazene-l,2-dicarboxylate (1.587 g, 7.85 mmol) were mixed in THF (20 mL) at 0 C, and then 4-chloro-3-hydroxy-5-nitrobenzamide (1 g, 4.62 mmol) was added. The reaction solution was maintained at RT for 16 hrs then the brown reaction solution was partitioned between sat. NaHCC (aq) and EtOAc. The organic layer was washed with brine, dried over MgSC , concentrated and purified on silica gel (20 %-80 % (3 : 1 EtOAc/EtOH) / Hexane, with 2% NH4OH; 330 g RediSep column). Desired fractions were combined and concentrated to give the title compound as a white solid (970 mg, 47 % yield). NMR (400 MHz, OMSO-de) delta ppm 8.30 (s, 1 H), 8.05 (d, J=1.77 Hz, 1 H), 7.88 (d, J=1.77 Hz, 1 H), 7.80 (s, 1 H), 4.28 (t, J=6.21 Hz, 2 H), 3.31 (br. s., 4 H), 2.48 (t, J=7.10 Hz, 2 H), 2.33 (t, J=4.94 Hz, 4 H), 1.96 (t, J=6.59 Hz, 2 H), 1.40 (s, 9 H). LCMS (LCMS Method K): Rt = 0.69 min, [M+H]+ = 443.4.

132710-90-8, The synthetic route of 132710-90-8 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; PESIRIDIS, George Scott; RAMANJULU, Joshi M.; TRAN, Jean-Luc; YANG, Jingsong; (157 pag.)WO2019/69275; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

78551-60-7, tert-Butyl 4-benzyl-3-oxopiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

78551-60-7, Preparation 46: (‘S)-2-[?S2S)-2-amino-l-hvdroxy-3-phenylpropyl”|-4-benzyl-3-oxo-piperazine-l- carboxylic acid t-butyl ester Step A: (S)-4-benzyl-2-|Tl S,2SV2-(dibenzylamino)-l-hvdroxy-3-phenylpropyl]-3-oxo-piperazine- 1-carboxylic acid t-butyl esterDsopropylamine (1.42 mL, 10.08 mmol) was dissolved in anhydrous tetrahydrofuran (10 mL) and the mixture was cooled to -78 C. n-butyl Miium (2.5 M n-hexane solution, 3.9 mL) was added dropwise to the resulting solution. The mixture was stirred for 5 min and then stirred on an ice bath for 30 min. The reaction mixture was cooled to -78 C, and a solution of t-butyl 4-benzyl- 3-oxopiperazine-l-carboxylate (B) (2.44 g, 8.40 mmol) in 15 mL of anhydrous tetrahydrofuran was added dropwise thereto, followed by stirring at that temperature for 1.5 hours. Thereafter, a solution of 2(S)-2-(dibenzylamino)-3-phenylpropanal (A) (2.99 g, 9.07 mmol) in anhydrous tetrahydrofuran (15 mL) was added to the reaction mixture which was gradually warmed to room temperature. After stirring at room temperature for 16 hours, the reaction was terminated with addition of water, followed by extraction with saturated ammonium chloride (aqueous) and diethyl ether. The organic layer was taken, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (EtOAc/n-Hex = 1/5) to afford the title compound (1.92 g, 24%).

The synthetic route of 78551-60-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; LG LIFE SCIENCES, LTD.; WO2009/38411; (2009); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

30459-17-7, 1-(4-Trifluoromethylphenyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Compounds 1a-l and compounds 15-19 were synthesized in the same reaction: In a dichloromethane solution (2-3 mL) of chloroacetylchloride(1.1 eq), a dichloromethane solution (8-10 mL) of the appropriate piperazine (1 eq) and triethylamine (2.5 eq) was added dropwise and the reaction mixture was stirred overnight at room temperature under a nitrogen atmosphere. The reaction mixture was evaporated and the residue was extracted with ethylacetate-brine. The organic layer was dried over Na2SO4 and chromatographed on silica preparative TLC to give the desired products.When the reaction was run for 2 h, compounds 1a-l were the mainproducts (>90%).

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

Reference：
Article; Papadopoulou, Maria V.; Bloomer, William D.; Rosenzweig, Howard S.; O’Shea, Ivan P.; Wilkinson, Shane R.; Kaiser, Marcel; European Journal of Medicinal Chemistry; vol. 103; (2015); p. 325 – 334;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

21655-48-1, cis-2,6-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,21655-48-1

A solution of 4e (732mg, 4.38mmol), HATU (2.50g, 6.57mmol) and DIEA (1.13g, 8.8mmol) in DMF (20mL) was stirred at r.t. for 0.5 hour, then added dropwise to a solution of 9a (l.Og, 8.8mmol) in DMF (50mL) under 0°C for 1 hour. After the reaction was complete, the mixture was evaporated and the residue was dissolved in DCM (50mL) and washed with sat. Na2C03. The organic layer was separated, dried over anhydrous MgS04 and evaporated to give 9b (808mg, 70percent).

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

Reference：
Patent; XCOVERY HOLDING COMPANY, LLC; LIANG, Congxin; WO2012/48259; (2012); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics