Month: May 2021

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.

Acetonitrile (560 ml) and potassium bicarbonate (8 gm) are added to 6- fluoro-i-methyM-oxo-y-CI-piperazinyO^H-CI .SKhiazetofS^-alquinoline-S- carboxylic acid (14 gm, obtained as per the processes described in examples 1 and 2) under stirring at 25 – 300C, the contents are cooled to 150C and then the solution of 4-bromomethyl-5-methyl-1 ,3-dioxolen-2-one (10 gm) in acetonitrile (140 ml) is added at 15 – 200C for 30 to 45 minutes. The contents are stirred for 25 hours at 25 to 300C, filtered and the resulting filtrate is distilled under vacuum. To the residue added acetonitrile (70 ml), cooled the mass to 200C and then stirred for 1 hour to 1 hour 30 minutes at 20 – 250C. Filtered the solid, washed the solid with 15 ml of chilled acetonitrile and then dried to give 16 gm of prulifloxacin crude (HPLC Purity: 98.8%).To the prulifloxacin crude (obtained above) added acetonitrile (200 ml) at 25 – 300C, the contents are heated to reflux and then refluxed for 30 minutes. To the reaction mass added activated carbon (5 gm) and refluxed for 15 minutes. The reaction mass is filtered on hi-flo bed, the resulting filtrate is cooled to 200C and then stirred for 3 – 4 hours at 20 – 250C. Filtered the solid, washed with 20 ml of acetonitrile and then dried to give 14 gm of prulifloxacin (HPLC Purity: 99.9%)., 112984-60-8

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 124225, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; HETERO DRUGS LIMITED; WO2008/59512; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

438631-77-7, (R)-1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 7-bromo-4,6-dichloro-3-nitroquinoline (4.97 g, 15.44 mmol) in THF (100 mL) was added 1-tert-butyl 3-methyl (3R)-piperazine-1,3-dicarboxylate (4.9 g, 20.07 mmol) followed by DIPEA (8.07 mL, 46.31 mmol) and reaction mixture heated at reflux overnight. Further 1-tert-butyl 3-methyl (3R)-piperazine-1,3-dicarboxylate (0.943 g, 0.25 eq) was added, along with further DIPEA (1.35 mL, 0.5 eq) and the reaction mixture heated at reflux for a further 24 h. The reaction mixture was partially concentrated and partitioned between water and EtOAc. Layers were separated, the organic layer washed with water and the combined aqueous layers were back extracted with EtOAc. The combined organic layers were dried (phase separator) and concentrated in vacuo to afford crude material as a dark brown oil. This was purified by flash silica chromatography (0 to 18% EtOAc in heptane) to afford 1-tert-butyl 3-methyl (3R)-4-(7-bromo-6-chloro-3-nitroquinolin-4-yl)piperazine-1,3-dicarboxylate (5.2 g, 64%) as an orange foam; 1H NMR (400 MHz, DMSO, 30 C.) 1.44 (9H, s), 3.29 (2H, s), 3.5-3.58 (3H, m), 3.6-3.69 (1H, m), 3.73 (1H, dd), 3.78-3.9 (1H, m), 4.02-4.2 (1H, m), 4.3-4.38 (1H, m), 8.49 (1H, s), 8.52 (1H, s), 9.11 (1H, s); m/z: ES+ [M+H]+ 529, 531.

438631-77-7, The synthetic route of 438631-77-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; Kettle, Jason Grant; Bagal, Sharanjeet; Robb, Graeme Richard; Smith, James Michael; Goldberg, Frederick Woolf; Cassar, Doyle Joseph; Feron, James Lyman; US2019/177338; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

13889-98-0, To a sealed tube was added 5-bromo-2-nitropyridine 111-1 (2.3 g, 11.4 mmol), l-(piperazin-l-yl)ethanone 111-2 (1.6 g, 12.8 mmol), triethylamine (4.8 mL, 34.2 mmol) and DMSO (5 mL). The reaction was heated to 120C and stirred for 16 hours. The reaction was cooled to room temperature. Triethylamine was removed by rotary evaporation. The residue was triturated in 15 mL ethyl acetate. The solid was collected by filtration and washed with small amount of ethyl acetate to give l-(4-(6-nitropyridin-3-yl)piperazin-l-yl)ethanone 111-3 as a light yellow solid. MS m/z 251.1 (M + 1).

The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; IRM LLC; CHENG, Dai; ZHANG, Guobao; HAN, Dong; GAO, Wenqi; PAN, Shifeng; WO2010/101849; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

694499-26-8, 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,694499-26-8

To a solution of 3-ethynyl-4-methylbenzoic acid (500 mg, 3.12 mmol, 1.05 eq) in DCM, HATU (1.42 g, 3.74 mmol, 1.2 eq) and DIPEA (806 mg, 6.24 mmol, 2.0 eq) was added. The mixture was stirred at room temperature for 30 min or so. Then to the solution 3-trifluoromethyl-4-[(4-methylpiperazin-1-yl) methyl]aniline (812 mg, 2.97 mmol, 1.0 eq) was added and the temperature was raised to 45 C. The reaction is completed after 20 h and the solvent was evaporated to dryness under reduced pressure to afford the residue extracted twice with DCM and saturated sodium bicarbonate aqueous solution. The DCM layer was evaporated to dryness to afford yellow oil which was purified by column chromatogram to give intermediate 74 as a yellowish brown solid (807 mg, 65.4% yield). 1H NMR (400 MHz, CDCl3) delta 8.33 (s, 1H), 7.91 (s, 1H), 7.86 (d, J=13.7 Hz, 2H), 7.73 (t, J=7.1 Hz, 2H), 7.28 (s, 1H), 3.60 (s, 2H), 3.32 (s, 1H), 2.48 (br.s, 11H), 2.30 (s, 3H). MS m/z (ESI): 416.3 [M+H].

694499-26-8 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline 46838908, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Si Chuan University; Yang, Shengyong; Wei, Yuquan; (168 pag.)US2017/305920; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

630125-91-6,630125-91-6, 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 4-Bromophenoxyacetic acid (1.20 g, 4.66 mmol) in anhydrous dichioromethane (10 mL) was added oxalyl chloride (0.59 g, 4.66 mmol)followed by a few drops of N,N-dimethylformamide at 0 C. After stirring at room temperature for one hour, a solution of 4-[(4-ethylpiperazin-1-yl)methyl]-3- (trifluoromethyl)aniline (2.50 g, 8.69 mmol) and triethylamine (2.63 g, 26.0 mmol) in anhydrous dichloromethane (10 mL) was added dropwise at 0 C and warmed to room temperature. After 16 h, the reaction mixture was partitioned between water (200 mL)and dichloromethane (100 mL). The aqueous layer was further extracted with dichloromethane (100 mL). The combined organic extracts were washed with brine (400 mL), dried (Na2SO4), the solvent evaporated and the residue purified by flash chromatography (Redisep silica gel, 97:3 CH2C12/MeOH) to afford 2-(4-bromophenoxy)- N- {4-[(4-ethylpiperazin- 1 -yl)methyl] -3 -(trifluoromethyl)phenyl } -acetamide (2.60 g). 1HNMR (400 MHz, DMSO-d6): 10.37 (s, 1H), 8.06 (s, 1H), 7.85-7.83 (dd, J= 8.4, 1.7Hz, 1H), 7.69-7.66 (a, J 8.5 Hz, 1H), 7.49-7.47 (d, J 9.2 Hz, 2H), 6.99-6.97 (d, J8.8 Hz, 2H), 5.75.(s, 2H), 4.72 (s, 2H), 3.53 (s, 2H), 2.37-2.27 (m, 1OH), 0.99-0.95 (t, J= 7.2 Hz, 3H); ESI MS, m/z 499 [M-H].

As the paragraph descriping shows that 630125-91-6 is playing an increasingly important role.

Reference：
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH (A*STAR); CHERIAN, Joseph; DURAISWAMY, Athisayamani Jeyaraj; NACRO, Kassoum; WO2014/88519; (2014); 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.13754-38-6,1-Benzoylpiperazine,as a common compound, the synthetic route is as follows.,13754-38-6

Manufacturing Example 10 1-(4-benzoylpiperazine-1-yl)propan-2-one 0.10 g (0.53 mmol) 1-benzoylpiperazine and potassium carbonate 0.22 g (1.58 mmol, 3.0 eq.) were added to 5 ml acetonitrile and 0.05 g (0.53 mmol, 1.0 eq.) chloroacetone was added dropwise slowly at room temperature. After mixing for one hour, 5 ml purified water was added, and the reaction mixture was extracted with 10 ml ethylacetate three times. After collecting organic layer, drying with anhydrous magnesium sulfate, and concentrating with decompression, residues obtained were purified with silicagel chromatography (mobile phase: dichloromethane/methnol=10:1) and 0.11 g (83%) target compound as yellow serup were yielded. 1H NMR (400 MHz, CDCl3) 2.18 (3H, s), 2.41-2.69 (4H, m), 3.27 (2H, s), 3.42-3.54 (2H, m), 3.81-3.93 (2H, m), 7.40-7.46 (5H, m)

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

Reference：
Patent; YANG JI CHEMICAL CO., LTD.; US2012/190689; (2012); 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.934-98-5,2-(4-Methylpiperazin-1-yl)ethanamine,as a common compound, the synthetic route is as follows.

General procedure: In a schlenk-type flask, a mixture of Pd2(dba)3 (0.023 g, 0.025mmol) and XantPhos (0.015 g, 0.025 mmol) in dry dioxane wasstirred at room temperature for 5 min. Then, NHR (2 mmol) andCs2CO3 (0.24 g, 0.75 mmol) were added and stirred for another 5min at ambient temperature. Afterwards, E-6 (F-4) (0.5 mmol)was added, and the flask was evacuated and backfilled with nitrogenfor three times. The reaction mixture was stirred at 100 C for9 h and followed by TLC until completion. After cooling, the solventwas removed under reduced pressure. The residue was purified byflash column chromatography with ethyl acetate/petroleum etherto afford compounds E-a?E-k (F-a?F-j). White solid, yield 31percent, mp: 144?146 C; 1H NMR (400 MHz,CDCl3) d: 7.51 (d, J = 1.6 Hz, 4H, PhH), 7.33 (d, J = 16 Hz, 1H, CH),7.20 (s, 2H, PhH), 6.96 (s, 1H, NH), 5.83 (d, J = 16.6 Hz, 1H, CH),5.62 (s, 1H, pyridine-H), 5.35 (s, 1H, pyridine-H), 3.34 (s, 2H,CH2), 2.80 (s, 4H, CH2), 2.68 (s, 2H, CH2), 2.45 (s, 3H, CH3), 2.14(s, 6H, CH3), 1.89 (s, 2H, CH2), 1.25 (s, 2H, CH2); 13C NMR (100MHz, CDCl3) d: 152.7, 149.8, 133.2, 132.3, 128.2, 117.9, 96.0,86.2, 51.7, 44.9, 16.3; ESI?MS: 508.2 [M+H+]. C30H33N7O (507.27)., 934-98-5

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Lu, Xueyi; Yang, Jiapei; Kang, Dongwei; Gao, Ping; Daelemans, Dirk; De Clercq, Erik; Pannecouque, Christophe; Zhan, Peng; Liu, Xinyong; Bioorganic and Medicinal Chemistry; vol. 26; 8; (2018); p. 2051 – 2060;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

883554-88-9, 4-Carbamoyl-piperazine-1-carboxylic acid tert-butyl ester is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The white solid from step A in ethanol (50 mL) was cooled to 0 C., and a pre-mixed solution of NaOCl (10-13% active chlorine, 43.4 mL) and 15% NaOH (78.0 mL) was added dropwise via an addition funnel. The ice bath was removed and the resulting mixture was stirred at room temperature for 1 h. 1N HCl was added to the resulting mixture until the pH of the solution was about pH 1, and the resulting mixture was stirred at room temperature for an additional 15 min. The pH of the solution was made basic with saturated aqueous potassium carbonate, and the resulting solution concentrated in vacuo to half the volume, then extracted three times with EtOAc, the combined organics were dried with Na2SO4, and concentrated in vacuo to yield the title compound, which was used in the next step without further purification. MS 202 (M+1)+, 883554-88-9

883554-88-9 4-Carbamoyl-piperazine-1-carboxylic acid tert-butyl ester 17750351, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; MACIELAG, Mark J.; Tennakoon, Manomi; US2009/275594; (2009); 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.55112-42-0,4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride,as a common compound, the synthetic route is as follows.

4-Methyl-l-piperazinecarbonyl chloride hydrochloride (19.9 mg, 0.1 mmol) was added to a solution of 4 (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 5 (23.6 mg, 91%). ?NMR DMSO-d6) 8 12.03 (s, 1H), 8.41 (s, 1H), 8.21 (s, 1H), 8.01 (d, 1H, J=8.4 Hz), 7.88 (d, 1H, J=8.4 Hz), 7.82 (dd, 1H, J=8.4 Hz), 7.58 (t, 1H, J=8.1 Hz), 7.51 (d, 1H, J=8.4 Hz), 7.46 (t, 1H, J=7.6 Hz), 7.37 (s, 1H), 4.86 (t, 1H, J=10.8 Hz), 4.57 (dd, 1H, J=10.8 Hz), 4.38 (m, 1H), 4.06 (dd, 1H, J=10.8 Hz), 3.86 (dd, 1H, J=11 Hz), 3.41 (br, 4H), 3.29 (br, 4H), 2.82 (s, 3H), 2.57 (s, 3H). Synthesis of Compound (7). A solution of 5 (13 mg, 24 umol) and linker 6 (16.9 mg, 31 umol) in 5% acetic acid in dry methylene chloride (1 ml) was stirred for 30 min at 25 C. The solvent was completely removed in vacuo and purified by HPLC (SymmetryPrep C18, 7mum, 19 x 150 mm column) to give 7 (18.5 mg, 81%). MS: calcd for C48H57ClN8O11 (M+H) m/z 958.38, found 958.10., 55112-42-0

The synthetic route of 55112-42-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; MEDAREX, INC.; WO2005/112919; (2005); 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.197638-83-8,1-Boc-4-(4-Formylphenyl)piperazine,as a common compound, the synthetic route is as follows.

Example 56 4-(4-tert-Butoxycarbonylpiperazin-1-yl)benzaldehyde 4-(oxazol-5-yl)phenylhydrazone 4-(4-tert-Butoxycarbonylpiperazin-1-yl)benzaldehyde (363 mg) was added to an ethanol solution (10 ml) of 4-(oxazol-5-yl)phenylhydrazine (200 mg), followed by heating overnight under reflux. Dichloromethane was added to the residue obtained by evaporating the solvent, and the thus precipitated solid was collected by filtration, washed with diethyl ether and then dried to obtain the title compound (427 mg) as a yellow solid. 1H-NMR (400 MHz, CDCl3) delta: 1.49 (9H, s), 3.21 (4H, bs), 3.58 (4H, bs), 6.91 (2H, d, J=8.8 Hz), 7.13 (2H, d, J=8.8 Hz), 7.26 (1H, s), 7.55 (2H, d, J=8.8 Hz), 7.57 (2H, d, J=8.8 Hz), 7.62 (1H, s), 7.66 (1H, s), 7.85 (1H, s). ESI-MS m/z: 448 (M+H)+.

197638-83-8, As the paragraph descriping shows that 197638-83-8 is playing an increasingly important role.

Reference：
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1612204; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics