Month: June 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.112257-24-6,1-Boc-3-Carbamoylpiperazine,as a common compound, the synthetic route is as follows.

tert-Butyl 4-(1-benzhydrylazetidin-3-yl)-3-carbamoylpiperazine-1-carboxylate A mixture of 1-benzhydrylazetidin-3-yl methanesulfonate (2.69 g, 8.5 mmol), K2CO3 (1.76 g, 12.8 mmol), tert-butyl 3-carbamoylpiperazine-1-carboxylate (1.95 g, 8.5 mmol) in CH3CN (40 mL) was stirred at reflux for 16 h. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (dichloromethane/methanol=50:1) to afford the desired product. (2.08 g, 54% yield).

112257-24-6, As the paragraph descriping shows that 112257-24-6 is playing an increasingly important role.

Reference：
Patent; Ren, Pingda; Liu, Yi; Li, Liansheng; Feng, Jun; Wu, Tao; US2014/288045; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5464-12-0,5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Under an atmosphere of nitrogen gas, l-(2-hydroxyethyl)-4-methylpiperazine (13.93 g) was added to a stirred mixture of 4-(6-chloro-2,3-methylenedioxyanilino)-7-fluoro- 5-tetrahydropyran-4-yloxyquinazoline (12.9 g), sodium te/t-pentoxide (9.87 g) and 1 ,2-diethoxyethane (37.5 ml). Water (1.34 g) and 1,2-diethoxyethane (25 ml) were added and the resultant reaction mixture was stirred and heated to 86°C for 18 hours. The reaction mixture was cooled to 5O0C and, under vacuum distillation at approximately 60 millibar pressure, approximately 50 ml of reaction solvent was distilled off. The reaction mixture was neutralised to pH 7.0 to 7.6 by the addition of a mixture of concentrated aqueous hydrochloric acid (36percent, 10 ml) and water (84 ml) at a rate that kept the temperature of the reaction mixture at a maximum of 6O0C. With the temperature of the reaction mixture being kept at 6O0C, the reaction mixture was extracted with ethyl acetate (225 ml). The organic solution was washed with water (50 ml). Water (25 ml) was added and, with the temperature being kept at 6O0C, the mixture was stirred for 10 minutes, then allowed to stand for 30 minutes and the aqueous layer was separated. The organic layer was concentrated to a volume of about 100 ml by distillation of solvent at about 9O0C under atmospheric pressure. The residual mixture was cooled during 1 hour to 450C and held at that temperature for 2 hours to allow crystallisation of product. The mixture was warmed briefly to 550C and then cooled during 4 hours to 180C EPO and held at that temperature for 1 hour. The crystalline precipitate was isolated by filtration and washed in turn with water (17 ml) and with toe’t-butyl methyl ether (17 ml). There was thus obtained 4-(6-chloro-2,3-piiethylenedioxyanilino)-7-[2-(4-methylpiperazin-l-yl)ethoxy]- 5-tetrahydropyran-4-yloxyquinazoline as a trihydrate (11 g; 88percent purity by HPLC using Method B, retention time 7.3 minutes); NMR Spectrum: (CDCl3) 1.65 (br s, 3H), 1.9-2.05 (m, 2H), 2.2-2.3 (m, 2H), 2.31 (s, 3H), 2.4-2.8 (m, 8H), 2.9 (m, 2H), 3.6-3.7 (m, 2H), 3.95-4.05 (m, 2H), 4.2-4.25 (m, 2H), 4.8 (m,lH), 6.05 (s, 2H), 6.55 (s, IH), 6.75 (d, IH), 6.85 (s, IH), 7.0 (d, IH), 8.55 (s, IH), 9.25 (s, IH).A portion (10 g) of the material so obtained was placed on a filter and dried at ambient temperature in a stream of dry nitrogen gas. The resultant material was dissolved at 6O0C in dry isopropanol (140 ml) whilst maintaining a dry nitrogen atmosphere. The solution was allowed to cool to ambient temperature and to stand under a dry nitrogen atmosphere for 2 days. The resultant crystalline solid was isolated by filtration under a dry nitrogen atmosphere. The material (8 g) so obtained was a crystalline anhydrous form of 4-(6-chloro-2,3-methylenedioxyanilino)-7-[2-(4-methylpiperazin-l -yl)ethoxy]- 5-tetrahydropyran-4-yloxyquinazoline, m.p. 142 to 1440C.

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/64217; (2006); 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.112984-60-8,6-Fluoro-1-methyl-4-oxo-7-(piperazin-1-yl)-1,4-dihydro-[1,3]thiazeto[3,2-a]quinoline-3-carboxylic acid,as a common compound, the synthetic route is as follows.

To a stirred solution of 6-fluoro-1-methyl-4-oxo-7-(piperazin-1-yl)-1H,4H- [1,3]thiazeto[3,2-a]quinoline-3-carboxylic acid (280 mg, 0.80 mmol) and triethylamine (0.3 ml , 2.16 mmol) in DMF(5 ml), compound C (570 mg, 1 mmol) was added and final solution was stuffed at room temperature for overnight. After completion, the solvent was evaporated, extracted with ethylacetate and washed with water. The organic extract was evaporated to obtain the crude mass which was further purified by flash column chromatography over silica gel using 2% methanol- DCM as eluent to obtain the compound D as an off white solid (220 mg, 48%). 1H NMR (DMSO-d6): 1H NMR (CDC13): isomer I: oe 14.66 (s,1H, COOH), 10.07 (s, 1H, NH), 8.66 (d, 1H, JAB= 1.5 Hz, ArH), 7.96 (s, 1H, ArH), 7.82 (d, 1H, JAB= 14.0 Hz, ArH), 7.70-7.66 (m, 1H, ArH), 6.95 (d, 1H, JAB= 7.0Hz, ArH), 6.40 (q, 1H, JAB = 6 Hz, SCHN), 3.44-3.37 (m, 4H, CH2N), 3.29 (s, 2H, CH2), 2.80-2.75(m, 4H, CH2N), 2.13 (d, 3H, JAB = 6.0 Hz, CH3), 1.64 (s, 9H, CH3), 1.36 (s, 18H, CH3); Isomer II: oe14.66 (s,1H, COOH), 10.01 (s, 1H, NH), 8.15 (d, 1H, JAB= 1.5 Hz, ArH), 7.90 (d, 1H, JAB= 9 Hz,ArH), 7.82 (d, 1H, JAB= 14.0 Hz, ArH), 7.70-7.66 (m, 1H, ArH), 7.51 (dd, 1H, JAB= 8.5 Hz, Jm= 1.5Hz,ArH), 6.95 (d, 1H, JAB= 7.0 Hz, ArH), 6.40 (q, 1H, JAB = 6 Hz, SCHN), 3.44-3.37 (m, 4H,CH2N), 3.29 (s, 2H, CH2), 2.80-2.75 (m, 4H, CH2N), 2.13 (d, 3H, JAB = 6.0 Hz, CH3), 1.64 (s, 9H,CH3), 1.36 (s, 18H, CH3)., 112984-60-8

The synthetic route of 112984-60-8 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; VYOME BIOSCIENCES PVT. LTD.; SENGUPTA, Shiladitya; GHOSH, Shamik; GHOSH, Sumana; SINHA, Mau; SADHASIVAM, Suresh; BHATTACHARYYA, Anamika; MAVUDURU, Siva Ganesh; TANDON, Nupur; KUMAR, Deepak; (149 pag.)WO2017/17631; (2017); 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.108-49-6,2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

Step 1 Synthesis of 3,5-Dimethyl-piperazine-1-carboxylic acid tert-butyl ester A solution of BOC-anhydride (374 mg, 1.71 mmol) in chloroform (2 mL) was added dropwise to a stirred solution of 2,5-dimethyl-piperazine (20 g, 266.5 mmol) in chloroform (2 mL) and the resulting mixture was stirred at room temperature for 4 hr. The reaction mixture was then diluted with cold water and extracted with chloroform, dried the organic layer over sodium sulfate and concentrated under reduced pressure to afford 331 mg (88.6percent yield) of 3,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester. LCMS Purity: 91.3percent., 108-49-6

The synthetic route of 108-49-6 has been constantly updated, and we look forward to future research findings.

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

55112-42-0, 4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,55112-42-0

4-Methyl-l-piperazinecarbonyl chloride hydrochloride (19.9 mg, 0.1 mmol) was added to a solution of 16 (20 mg, 0.05 mmol) and anhydrous pyridine (25 muml, 0.3 mmol) in 3% allyl alcohol in dry methylene chloride (4 ml) and the mixture was stirred for 16 h. Purification of the crude product on silica gel yielded 17 (23.6 mg, 91%). 1NMRDMSOd6) delta 12.03 (s, IH), 8.41 (s, IH), 8.21 (s, IH), 8.01 (d, IH, J=8.4 Hz), 7.88 (d, IH, J=8.4 Hz), 7.82 (dd, IH, J=8.4 Hz), 7.58 (t, IH, J=8.1 Hz), 7.51 (d, IH, J=8.4 Hz)5 7.46 (t, IH, J=7.6 Hz), 7.37 (s, IH), 4.86 (t, IH, J=10.8 Hz), 4.57 (dd, IH, J=10.8 Hz), 4.38 (in, IH), 4.06 (dd, IH, J=I 0.8 Hz), 3.86 (dd, IH, J=I 1 Hz), 3.41 (br, 4H), 3.29 (br, 4H), 2.82 (s, 3H), 2.57 (s, 3H).

55112-42-0 4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride 3016934, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; MEDAREX, INC.; WO2007/51081; (2007); 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

p-Nitrophenyl chloroformate (4.16 g) and pyridine (2.0 mL) were added to a solution of N-tert-butyloxycarbonyl-N’-(4-aminophenyl)-piperazine (5.54 g) in anhydrous tetrahydrofuran (40 mL) at 0C. The reaction mixture was stirred at 0C for one hour and stirred at room temperature for three hours and diluted with 1N hydrochloric acid, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium hydrogen carbonate aqueous solution and saturated brine, dried over sodium sulfate and concentrated. The obtained solid was collected by filtration and dried and 6.42 g (72%) of the title compound was obtained as a pale yellow solid. 1H NMR(400MHz,DMSO-d6):delta(ppm)=8.26(2H, d, J=9.OHz), 7.37(2H, d, J=9.0Hz), 7.34(2H, d, J=9.OHz), 6.97(IH, brs), 6.92(2H, d, J=9.OHz), 3.58(4H, t, J=5.1Hz), 3.10(4H, t, J=5.1Hz), 1.48(9H, s).

170911-92-9, The synthetic route of 170911-92-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Sankyo Company, Limited; EP1764360; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

259808-67-8, 1-Boc-3,3-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 27 (1.00 g, 4.6 mmol) in CH2C12 (10 mL) at0C was charged with Et3N (2.30 g, 23 mmol) followed by MsC1 (0.59 mg, 7.0 mmol). The reaction mixture was stirred at room temperature for 2 h. Water (50 mL) was added to the reaction mixture and extracted with CH2C12 (2 x 50 mL). The organic phase was separated, dried over anhydrous Na2504, filtered and concentrated to afford 28 [1.20 g (cmde)j as a solid, whichwas used for the next step without further purification.

259808-67-8, 259808-67-8 1-Boc-3,3-Dimethylpiperazine 22710387, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; IOMET PHARMA LTD.; MERCK SHARP & DOHME CORP.; COWLEY, Phillip, M.; WISE, Alan; BROWN, Thomas, J.; MCGOWAN, Meredeth, A.; ZHOU, Hua; HAN, Yongxin; (223 pag.)WO2017/7700; (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.5747-48-8,11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine,as a common compound, the synthetic route is as follows.

Compound 12(20.00 gm, 67.71 mmol), Boc protected Phenyl alanine (19.75 gm, 74.46 mmol),TBTU (32.61 gm, 101.57 mmol), DMF (200 mL, 10 Vol) and DIPEA (26.25 gm, 203.13mmol) were taken in a round bottom flask at room temperature under nitrogenatmosphere. The reaction was stirred for 12 hours at the same temperature and then monitored by TLC. After completion of thestarting material the reaction mixture was diluted with water (600 mL) andstirred for 1 hour at room temperature. The solids were filtered and washedwith water (100 mL x 2) and then dried under vacuum at 50 C to yield 30 gof Compound13 (Yield 82%) as an off-white solid. Offwhite solid; m.p. 120-124 C; 1H NMR (400 MHz, DMSO-d6): delta 7.54-7.56(d, 1H, J=8.0 Hz), 7.42-7.47 (m,4Hz), 7.17-7.25 (m, 7H), 6.98-7.00 (d, 1H, J=8.0Hz), 6.88-6.92 (1H, t, J=7.6 Hz),4.58-4.60 (d, 1H, J=7.2 Hz),3.44-3.82 (m, 6H), 3.11-3.19 (bs, 1H), 2.75-2.90 (m, 3H) and 1.30 (s, 9H); Massm/z = 543 (M+H)+., 5747-48-8

Big data shows that 5747-48-8 is playing an increasingly important role.

Reference：
Article; Gudisela, Mura Reddy; Srinivasu; Mulakayala, Chaitanya; Bommu, Praveen; Rao, M.V. Basaveswara; Mulakayala, Naveen; Bioorganic and Medicinal Chemistry Letters; vol. 27; 17; (2017); p. 4140 – 4145;,
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.120737-59-9,tert-Butyl 3-methylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

General Procedure: To a 75 mL screw-cap round bottom flask equipped with a stir bar were added l-bromo-2,4-dichlorobenzene (0.72 mL, 5.99 mmol), 3-methyl-piperazine-l-carboxylic acid tert-butyl ester (1.0 g, 4.99 mmol), 2-di-tert-butylphosphino-2′-(N,N- dimethylamine)biphenyl (51.1 mg, 0.15 mmol), tris(dibenzylideneacetone)dipalladium (45.7 rag, 0.05 mmol) and tetrahydrofuran (30 mL). The reaction flask was flushed with nitrogen for 5 minutes and then lithium bis(trimethylsilyl)amide (1 M in tetrahydrofuran, 6.99 mL, 6.99 mmol) was added in one portion. The reaction flask was sealed and the reaction mixture was stirred at room temperature for 72 hours. The reaction mixture was concentrated in vacuo and the residue purified on silica gel using hexanes: acetone = 98:2 to give the desired product as an off-white solid (130 mg, 8 percent). 1H NMR (300 MHz, CDCl3): delta 6.77 (t, IH)5 6.68 (d, 2H)5 4.10 (bs, IH), 3.85 (bss 2H), 3.12 (m, 4H). 1.48 (s, 9H), 1.04 (d, 3H).

120737-59-9, The synthetic route of 120737-59-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2007/87135; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

115761-79-0, 1-(2,4-Difluorophenyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: To a stirred solution of 3 (4, 5) (0.10 mmol) in DMSO (10 ml) were added ZH (0.12 mmol) and K2CO3 (27.6 mg 0.20 mmol). After stirring at 80 C for 8 hours, the mixture was cooled to room temperature and poured into water, the precipitation was filtered and dried directly for next step. To a solution of above solid (0.10 mmol) in dry THF (10 ml) was added LiAlH4 (11.4 mg, 0.30 mmol) at 0 C. After stirring at room temperature for 4 h, the mixture was quenched with water and extracted by CH2Cl2 (10 ml). The extraction was dried over anhydrous MgSO4 and filtered. The filtration was concentrated for next step. To a solution of above crude solid (0.12 mmol) in dry CH2Cl2 (10 ml) were added compound 6 (7-11) (0.10 mmol), TEA (22.2mg, 0.22 mmol) and BopCl (30.4 mg, 0.12 mmol). After stirring at room temperature for 12 h, the mixture was washed with brine and dried over anhydrous MgSO4, filtered and concentrated. The residue was purified by silica gel column (CH2Cl2 : MeOH = 100 : 1) to yield compounds 1, 2, A, B, C., 115761-79-0

115761-79-0 1-(2,4-Difluorophenyl)piperazine 2734637, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Wang, Hongjian; Lv, Kai; Li, Xiaoning; Wang, Bo; Wang, Apeng; Tao, Zeyu; Geng, Yunhe; Wang, Bin; Huang, Menghao; Liu, Mingliang; Guo, Huiyuan; Lu, Yu; Chinese Chemical Letters; vol. 30; 2; (2019); p. 413 – 416;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics