Month: August 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.132710-90-8,1-Boc-4-(3-hydroxypropyl)piperazine,as a common compound, the synthetic route is as follows.

Triphenylphosphine (2.059 g, 7.85 mmol), tett-butyl 4-(3-hydroxypropyl)piperazine-1-carboxylate (1.692 g, 6.93 mmcl) and diisopropyl (E)-diazene-1,2-dicarboxylate (1.587 g, 7.85mmcl) were mixed in THE (20 mL) at 0 C, and then 4-chloro-3-hydroxy-5-nitrobenzamide (1 g, 4.62 mmcl) was added. The reaction solution was maintained at RT for 16 hrs then the brown reaction solution was partitioned between sat. NaHCO3 (aq) and EtOAc. The organic layer was washed with brine, dried over Mg504, concentrated and purified on silica gel (20 %80 % (3:1 EtOAc/EtOH) I 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). 1H NMR (400 MHz, DMSO-d6) 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 Ct, J=4.94 Hz, 4 H), 1.96 Ct, J=6.59 Hz, 2 H), 1.40 Cs, 9 H). LCMS CLCMS Method K):Rt = 0.69 mm, [M+H] = 443.4.

132710-90-8, 132710-90-8 1-Boc-4-(3-hydroxypropyl)piperazine 16217800, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CHARNLEY, Adam Kenneth; DARCY, Michael Gerard; DODSON, Jason W.; DONG, Xiaoyang; FAVRE, David; HUGHES, Terry Vincent; KANG, Jianxing; LEISTER, Lara Kathryn; LI, Yuehu; LIAN, Yiqian; MEHLMANN, John F.; NEVINS, Neysa; RAMANJULU, Joshi M.; ROMANO, Joseph J.; WANG, Gren Z.; YE, Guosen; ZHANG, Daohua; (489 pag.)WO2019/69269; (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.182618-86-6,1-Boc-4-(4-Nitrophenyl)piperazine,as a common compound, the synthetic route is as follows.

To the reaction flask was added compound 40 (17.57 g, 63.39 mmol)Soluble in methanol,Add 1.7 g of Pd / C,Catalytic hydrogenation at room temperature,TLC tracking, to be completely complete,Diatomaceous earth filtration,The solvent was removed by distillation under reduced pressure,To obtain a crude solid,And then beaten with ether to get pink powder,Drying to give 12.31 g of compound 7-11,Yield: 73.8%., 182618-86-6

The synthetic route of 182618-86-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Zhengda Tianqing Pharmaceutical Group Co., Ltd.; Zhang Yinsheng; Gao Yong; Ren Jing; Wang Qinglin; Wang Zhao; (67 pag.)CN106905245; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

163765-44-4, (R)-1-Boc-3-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

163765-44-4, The compound (R) -3- methyl-piperazine-1-carboxylate (250mg, 1.25mmol), cyclopropanecarboxylic acid(130mg, 1.50mmol), 1- Ethyl-3- (3-dimethylaminopropyl) carbodiimide hydrochloride (480mg, 2.50mmol)and N- hydroxy-7-aza-benzotriazole (254mg, 1.87 mmol) were dissolved in dichloromethane (10 mL), and theconditions under 0 C, to this solution was added dropwise N, N- diisopropylethylamine (0.65mL, 3.74mmol), stirred for 10H at room temperature, add water (10mL × 3) washing the organic phase was dried overanhydrous Na 2 SO 4, the solvent was removed, the concentrate was subjected to column Chromatography(eluent: Petroleumether / EtOAc (v / v) = 2/1), to give 310mg of colorless liquid: (R) -4- (cyclopropylcarbonyl)-3- Methyl-piperazine-1-carboxylate, yield: 93%.

163765-44-4 (R)-1-Boc-3-Methylpiperazine 2756811, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Guangdong East Sunshine Pharmaceutical Co., Ltd; Zhang, Ying jun; Liu, Bing; Yu, Tian Zhu; Zhang, Xiang Yu; (348 pag.)CN105399698; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

169448-87-7, (R)-tert-Butyl 2-(hydroxymethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

a) A mixture of (R)-6-bromo- l-(l-(2,4-dichlorophenyl)ethyl)- lH-indazole (prepared from Example 17 step c, 0.37 g, 1.0 mmol), (i?)-i-butyl 2- (bydroxymeihy])piperidirie~1 -carboxylase (0.22 g, 1.0 mmol), BetaGammaNuAlphaRho (0.093 g, 0.15 mmol), and CS2CO3 (0.65 g, 2.0 mmol) in toluene (1 mL) was purged with nitrogen for 5 min. Addition of Pd2(dba)3 (0.092 g, 0.10 mmol) was followed, and the mixture was purged with nitrogen for 1 min. The reaction was then heated at 100 C for 18 h. After cooling to room temperature, the mixture was filtered and washed with EtOAc (50 mL). The filtrate was concentrated in vacuo. The resulting crude mixture was purified by flash chromatography (S1O2, 40% ethyl acetate in hexanes) to afford the coupled product as a viscous oil (0.20, 0.40 mmol, 40%)., 169448-87-7

The synthetic route of 169448-87-7 has been constantly updated, and we look forward to future research findings.

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

314741-40-7, (S)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a flask was added benzyl 5-bromoisoindoline-2-carboxylate (compound 3a, 200 mg, 602 pmol), ZerZ-butyl (3.S’)-3-(hydroxymethyl)piperazine- 1 -carboxylate (CAS: 314741-40-7, Vendor: PharmaBlock, 195 mg, 903 pmol), sodium ZerZ-butoxide (116 mg, 1.20 mmol) and 1,4- dioxane (4 mL), the suspension was bubbled with N2 for 5 mins and Z-BuXPhos Pd G3 (48 mg, 60 pmol) was added. The mixture was heated at 90 C under microwave for 2 hrs. After being cooled down, the mixture was diluted with EA (10 mL) and filtered through celite. The filtrate was concentrated to give a brown oil which was purified by flash column (MeOH/DCM = 0 to 10%) to give compound 3b (183 mg) as a light yellow oil. MS: calc?d 468 (MH+), measured 468 (MH+).

314741-40-7, 314741-40-7 (S)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate 24820294, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DEY, Fabian; KOU, Buyu; LIU, Haixia; SHEN, Hong; WANG, Xiaoqing; ZHANG, Weixing; ZHANG, Zhisen; ZHANG, Zhiwei; ZHU, Wei; (203 pag.)WO2019/238616; (2019); 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

Intermediate 28: Piperazine-1-carboxylic acid amide hydrochloride; [] 4-Piperazine-1-carboxylic acid tert-butyl ester (1.0g, 5.4mmol), acetic acid (3ml) and water (5ml) were mixed together. Potassium cyanate (2.25g, 27.7mmol) was added portionwise as a solution in water (5ml) and stirred for 4 hours, during which time a solid precipitated. The solid was filtered, re-dissolved in DCM (20ml), dried over MgSO4, filtered, the filter cake washed with DCM (5vol) and concentrated in vacuo to give a white solid (0.38g). The white solid (0.38g) was dissolved in methanol (3.8ml) and 1,4-dioxane (0.7ml), 4M HCl in 1,4-dioxane (2.5ml, 10mmol) was added to the reaction and stirred overnight. The reaction was concentrated in vacuo to give the title compound (0.28g, 31% over 2 steps) as a white solid.1H NMR (400MHz, DMSO-d6) delta9.18 (br s, 2H), 3.91 (br s, 2H), 3.45 (br s, 4H), 2.93 (br s, 4H)., 57260-71-6

The synthetic route of 57260-71-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Warner-Lambert Company LLC; EP1593679; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

129722-25-4, 7-(4-(4-(2,3-Dichlorophenyl)piperazin-1-yl)butoxy)quinolin-2(1H)-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of dehydro-aripiprazole (1.50 g, 3.36 mmol), triethylamine (1.03 mL, 7.39 mmol), diethyl carbamoyl chloride (1.02 mL) were combined in tetrahydrofuran (30 mL). This was then heated to 100 C. for 6 hours by microwave. The reaction was quenched with water (50 mL) and extracted with dichloromethane (2×100 mL). The combined organics were dried (MgSO4) and concentrated. The crude product was purified by column chromatrography on silica eluting with ethyl acetate to 20% tetrahydrofuran/ethyl acetate to give the product. The product was then triturated with heptane to remove aliphatic impurities and then dried to give Compound 334 (1.54 g) as a light brown oil.1H-NMR (300 MHz, CDCl3) delta 8.10 (1H, d), 7.69 (1H, d), 7.31 (1H, d), 7.16-7.07 (4H, m), 6.99-6.92 (1H, m), 4.12 (2H, t), 3.54-3.39 (4H, 2×q), 3.12-2.96 (4H, br s), 2.78-2.54 (4H, br s), 2.50 (2H, t), 1.97-1.62 (4H, m), 1.32-1.16 (6H, 2×t). [M+H]+=545.2.

129722-25-4, As the paragraph descriping shows that 129722-25-4 is playing an increasingly important role.

Reference：
Patent; Alkermes, Inc.; US2011/319422; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

278788-66-2, (R)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step D: tert-butyl (3R)-4-[2-(3-cyano-4-fluorophenyl)-2-oxoethyl]-3-(hydrox)’Ilethyl)piperazine-1-carboxylate; To a solution of5-(bromoacetyl)-2-fluorobenzonitrile (13.1 g, 0.054 mol) inDMF (160 mL) was added tert-butyl (3R)-3-(hydroxymethyl)piperazine-1-carboxylate (13.1 g,0.065 mol) and K2C03 (11.77 g, 0.075mol), and the mixture was stirred at RTfor 3 h. Themixture was washed with water, and extracted with EtOAc. The organic layer was washed withbrine, dried over Na2S04 and concentrated in vacuum to give the title compound which was used for the next step without further purification., 278788-66-2

As the paragraph descriping shows that 278788-66-2 is playing an increasingly important role.

Reference：
Patent; MERCK SHARP & DOHME CORP.; PASTERNAK, Alexander; BLIZZARD, Timothy; CHOBANIAN, Harry; DE JESUS, Reynalda; DING, Fa-Xiang; DONG, Shuzhi; GUDE, Candido; KIM, Dooseop; TANG, Haifeng; WALSH, Shawn; PIO, Barbara; JIANG, Jinlong; WO2013/28474; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

78818-15-2, Benzyl 3-oxopiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

78818-15-2, Step C Preparation (+-)-4-Benzyloxycarbonyl-1-[1-(3-(benzyloxy)phenyl)-3-buten-1-yl]-2-piperazinone Sodium hydride (1.20 g, 30.0 mmol, 60% mineral oil dispersion) was triturated with hexane. The flask was charged with 15 mL of dimethylformamide and cooled to 0 C. 4-Benzyloxycarbonyl-2-piperazinone was added (4.55 g, 19.4 mmol), and the reaction was stirred for 15 minutes at 0 C. A solution of the product from Step B (4.83 g, 14.5 mmol) in 15 mL of dimethylformamide was added slowly, and the reaction was allowed to warm to room temperature. After 3 days, the solution was concentrated in vacuo, and partitioned between EtOAc and saturated NaHCO3 solution. The aqueous phase was extracted with EtOAc, and the combined organics were washed with saturated NaHCO3 soln and brine, dried (Na2SO4), filtered, and concentrated in vacuo. The resulting product was purified by silica gel chromatography (10% EtOAc/hexane, then 5% MeOH/CH2Cl2) to provide the titled product as a yellow oil.

The synthetic route of 78818-15-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Merck & Co., Inc.; US6562823; (2003); B1;,
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

In 35 mL of N,N-dimethylformamide were dissolved benzyl 1-piperazinecarboxylate (5.00 g, 22.7 mmol) and cyclopropanecarboxylic acid (2.54 g, 29.5 mmol), and 1-ethyl-3-(3-(N,N-dimethylamino)propyl)-carbodiimide hydrochloride (6.53 g, 34.1 mmol), 1-hydroxybenzotriazole (4.52 g, 29.5 mmol) and triethylamine (3.60 g, 35.9 mmol) were added thereto at room temperature, followed by stirring at the same temperature for three hours. The reaction mixture was mixed with water, and extracted twice with ethyl acetate. The organic layer was sequentially washed with water twice, with a saturated aqueous solution of sodium bicarbonate once and with brine once, and then dried over anhydrous sodium sulfate. The organic layer was passed through a silica gel column (Fuji Silysia, NH Silica gel) and evaporated to give the title compound (6.10 g, 93.1percent) as a white amorphous.1H-NMR Spectrum (CDCl3,400MHz) delta(ppm): 0.75-0.83(2H,m), 0.95-1.03(2H,m),1.65-1.75(1H,m),3.40-3.80(8H,m),5.16(2H,s), 7.30-7.40(5H,m)., 31166-44-6

As the paragraph descriping shows that 31166-44-6 is playing an increasingly important role.

Reference：
Patent; MERCIAN CORPORATION; Eisai Co., Ltd.; EP1508570; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics