Month: May 2021

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The chloropteridine from above was dissolved in n-butanol (50 mL) and N-methyl- N’-(2-aminoethyl)piperazine (2.0 gm, 1.4 X 10″2 moles) was added. This mixture was heated at 110°C. for 30 minutes. TLC (silica, 25percent methanol in methylene chloride) showed a single, blue fluorescent, product at Rf = 0.093. The n-butanol was removed under reduced pressure and the residual material was extracted by stirring in diethyl ether (50 mL). This mixture was filtered and the solid filtercake was washed with diethyl ether (100 mL). The combined filtrates were extracted with water (50 mL). These aqueous extracts were treated with potassium carbonate to precipitate the product as an oil. The product was extracted into methylene chloride (100 mL). After drying over magnesium sulfate the methylene chloride solution was filtered and evaporated under reduced pressure. The remaining solid (1.28 gm) was dissolved in methanol (40 mL) and the solution was heated to reflux. Concentrated hydrochloric acid (982mu) was added and the solution was cooled on ice. The hydrochloride salt of Example 57 crystallized and was isolated by filtration. After being washed with methanol followed by diethyl ether, the solid was dried to give the product as its hydrochloride salt in a yield of 950 mg. LC/MS: M+l = 448.45, 934-98-5

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; JANUS BIOTHERAPEUTICS, INC.; LIPFORD, Grayson, B.; ZEPP, Charles, M.; WO2012/167046; (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.162046-66-4,4-(4-(tert-Butoxycarbonyl)piperazin-1-yl)benzoic acid,as a common compound, the synthetic route is as follows.

A mixture of compound 3 (306 mg, 1 mmol), tert-butyl 2-amino-4-(thiophen-2-yl)phenylcarbamate (260 mg, 0.9 mmol) and 1 -(3-dimethylaminopropyl)-3-ethylcar- bodiimide hydrochloride (573 mg, 3 mmol) in pyridine (15 mE) was stirred at room temperature for overnight. The mixture was poured into water (100 mE), filtered to obtain compound 4 (442 mg, 85%) as a yellow solid., 162046-66-4

162046-66-4 4-(4-(tert-Butoxycarbonyl)piperazin-1-yl)benzoic acid 2795508, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Regenacy Pharmaceuticals, LLC; van Duzer, John H.; Mazitschek, Ralph; (123 pag.)US2018/141923; (2018); 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.31166-44-6,1-Cbz-Piperazine,as a common compound, the synthetic route is as follows.

Into a 100-mL round-bottom flask, purged and maintained with an inert atmosphere of nitrogen, was added tert-butyl (4-bromophenethyl)carbamate (4,00 g, 13.3 mmol) and anhydrous toluene (50 mL). To the resulting solution was added benzyl piperazine-1- carboxylate (3.53 g, 16.0 mmol), Pd(OAc)2 (300 mg, 1.34 mmol), XPhos (1.28 g, 2.69 mmol), and CsiCO, (13.1 g, 40.0 mmol). The reaction mixture was stirred overnight at 105 °C in an oil bath and then cooled to RT and quenched by the addition of H20 (200 mL). The resulting mixture was extracted with ethyl acetate (2 x 50 mL). The combined organic layers were washed with brine (1 x 200 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The crude product was purified by FCC eluting with ethyl acetate/petroleum ether (PE/EA=3 : 1) to afford benzyl 4-(4-(2-((fert-butoxycarbonyl)amino)ethyl)phenyl)piperazine-l- carboxylate as a yellow solid (5 g, 85percent), LCMS (ESI, m/z) 440 [M+H]+

31166-44-6, The synthetic route of 31166-44-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; FORMA THERAPEUTICS, INC.; GUERIN, David Joseph; BAIR, Kenneth W.; CARAVELLA, Justin A.; IOANNIDIS, Stephanos; LANCIA, JR., David R.; LI, Hongbin; MISCHKE, Steven; NG, Pui Yee; RICHARD, David; SCHILLER, Shawn E.R.; SHELEKHIN, Tatiana; WANG, Zhongguo; (113 pag.)WO2017/139779; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 1: Preparing gatifloxacin from compound (II) 10 g (0.0339 moles, 1 equivalent) of compound (II) is placed in a flask, 30 ml of acetonitryl (3 volumes) is added and this is heated to a temperature of 76-80 C. Once reflux has been attained, and being the temperature maintained, 3.28 g (0.0203 moles, 0.6 equivalents) of hexamethyldisilazane (HMDS) is added with a compensated adding funnel. Once addition is completed, the reaction is maintained with stirring for 1 hour at a temperature of 76-80 C. Once this period has elapsed, the reaction mixture is cooled to a temperature ranging between 0 and 15 C, and 5.78 g (0.0407 moles, 1.2 equivalents) of boron trifluoride ethyletherate is added while keeping the temperature below 15 C. Once addition is completed, the temperature is allowed to rise to 15- 25 C and it is kept under these conditions for approximately 2 hours. The pH of the mixture is then adjusted to an approximate value of 9 with triethylamine (approximately 2 ml). To the resulting suspension is added a solution of 10.19 g (0.1017 moles, 3 equivalents) of 2-methylpiperazine in 28 ml of acetonitryl, while maintaining the temperature between 15 and 25 C. The resulting amber solution is kept with stirring under these conditions for approximately 3 hours. Once the reaction has been completed, the solution is distilled at low pressure until a stirrable paste is obtained. At this point 50 ml of methanol is added, the resulting suspension is raised to a temperature of 63-67’C and is kept under these conditions for approximately 5 hours. Once the reaction has been completed, the mixture is cooled to a temperature of 25-35 C in a water bath, and then at a temperature of 0-5 C in a water/ice bath for a further 1 hour. The resulting precipitate is filtered, washed with cold methanol (2 x 10 ml) and dried at 40 C in a vacuum oven to constant weight. 10.70 g of crude gatifloxacin is obtained, having a water content of 2. 95% by weight. The yield of the process is 81. 8%. The crude product is crystallised in methanol by dissolving 20 g of crude gatifloxacin in 1 1 of methanol (50 volumes) at a temperature of 63-67 C. Once all the product has been dissolved, the solution is left to cool to a temperature of 30-40 C, and then to a temperature of 0-5 C in a water/ice bath, maintaining it under these conditions for 1 hour. The resulting suspension is filtered and the solid retained is washed with 20 ml (1 volume) of cold methanol. The solid obtained is dried at 40 C in a vacuum oven to provide 18.65 g of gatifloxacin with a water content of 2. 36% by weight. The overall yield from the compound (II) is 77. 7%, with a purity exceeding 99. 8% as determined by HPLC chromatography. The content of by-product resulting from demethylation in position 8 of the ring is lower than 0. 1% as determined by HPLC chromatography., 109-07-9

The synthetic route of 109-07-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; QUIMICA SINTETICA, S.A.; WO2005/47260; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step-III: Levorotatory (-)-[2-[4-[(4-Chlorophenyl)-phenylmethyl]-1-piperazinyl]ethanolLevorotatory (-)-1-[(4-chlorophenyl)phenylmethyl]piperazine (50 gm), 2-chloroethanol (31.4 gm), potassium iodide (1.3 gm) and sodium carbonate (40.8 gm) are taken in toluene (446 ml) and refluxed for 24 hours. The reaction mixture is cooled to 25-35 C., washed with water (285 ml) followed by two times with water (each time 185 ml). The layers are separated. Toluene is evaporated from organic layer under reduced pressure to yield 58 gm of levorotatory (-)-[2-[4-[(4-Chlorophenyl)-phenylmethyl]-1-piperazinyl]ethanol.

300543-56-0, 300543-56-0 (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine 668697, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; SYMED LABS LIMITED; US2009/281318; (2009); 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

2-chloro-6-fluoro-3-(oxiran-2-yl)benzonitrile (9.1 g, 46 mmol) and (R)-tert-butyl 3-(hydroxymethyl)piperazine-1-carboxylate (14.9 g, 69.1 mmol) were dissolved in ethanol (105 mL) and dispensed into 9 sealed tubes thenmicrowaved at 140C for 1 h. The combined reaction mixture was concentrated and purified through a 330g ISCORedi-sep column with 50%-100 ethyl acetate/hexane solvent system to yield the title compound., 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; (128 pag.)EP2744499; (2016); B1;,
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.694499-26-8,4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline,as a common compound, the synthetic route is as follows.

7-Bromo-1-methyl-1H-indole-2-carboxylic acid (2.5 g, 10 mmol), 4-((4-methylpiperazin-1-)methyl)-3-(trifluoromethyl) Aniline (2.73g, 10mmol) and2-(7-Oxobenzotriazole)-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HATU) (3.8 g, 10 mmol)Dissolved in N,N-dimethylformamide, added diethyl isopropylamine (1.65 mL, 10 mmol), stirred until the reaction was completed.Extracted with ethyl acetate and water, the organic phase was concentratedColumn chromatography gave product 3.6 g, yield 70%., 694499-26-8

As the paragraph descriping shows that 694499-26-8 is playing an increasingly important role.

Reference：
Patent; Beijing Seth Ming Qiang Pharmaceutical Technology Co., Ltd.; Zhang Qiang; Zhang Hongbo; Zhou Likai; Feng Shouye; Yang Hailong; Wang Zhongxiang; (54 pag.)CN109988151; (2019); A;,
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.154590-35-9,tert-Butyl 4-(4-amino-2-fluorophenyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Step 1: To the product of Preparation 13, Step 3 (1.00 g, 3.3 mmol) and DIPEA (0.88 ml, 5.1 mmol) in CH2Cl2 (15 ml) add trifluoroacetic anhydride (0.57 ml, 4.1 mmol). Stir 2 h and add a second portion each of DIPEA and anhydride. Stir 1 h and wash with satd. NaHCO3, then water. Dry (MgSO4) and concentrate to obtain the amide as a yellow solid, 154590-35-9

The synthetic route of 154590-35-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Schering Corporation; US2004/220194; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

169447-70-5, (S)-tert-Butyl 2-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To 1 ,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate (1g) in DCM (5OmL) was added DIPEA (1.74ml_). 4-cyanobenzenesulfonyl chloride (1.1g) was then added slowly and the reaction mixture was stirred for 1 hour. To the reaction was added DCM (5OmL) and the solution was washed with saturated sodium bicarbonate solution and water. The organic layer was collected and evaporated to dryness under vacuum. The resulting oil was dissolved in 1 ,4-dioxane (1OmL) before the addition of 4M HCI in 1 ,4-dioxane (1OmL) and a few drops of water. The reaction was stirred for 1.5 hours. The reaction mixture was evaporated to dryness under vacuum then dissolved in MeOH. The MeOH solution was loaded onto a 1Og SCX column. The loaded column was then washed with 2 column volumes of MeOH and the desired product was eluted from the column with 1 M ammonia in MeOH. The fraction containing eluted product was evaporated to dryness under vacuum to yield the title compound as a yellow oil (895mg, 68%).MS ES+ve m/z 265 (M+H)

169447-70-5, As the paragraph descriping shows that 169447-70-5 is playing an increasingly important role.

Reference：
Patent; GLAXO GROUP LIMITED; BESWICK, Paul, John; CAMPBELL, Alister; CRIDLAND, Andrew; GLEAVE, Robert, James; PAGE, Lee, William; WO2010/102663; (2010); 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.215309-01-6,3-(4-Methylpiperazin-1-yl)benzoic acid,as a common compound, the synthetic route is as follows.

Example 33: lambdaP-(2<:yano-9-methyl-9Hphiurin-6-yl)-lambdaP<:yclopentyl-3-(4-methyl-1 - piperazinyl)benzohydrazide trifluoroacetate.Intermediate 51 (2 g, 9.08 mmol) was dissolved in oxalyl chloride (2OmL) and the mixture was stirred overnight. The solvent was removed under reduced pressure and part of the residue (1.1 g, 4.64 mmol) was added to a solution of Intermediate 16 (300 mg, 1.16 mmol) and DIPEA (FLUKA, 0.794 mL, 4.64 mmol) in THF (50 mL). Potassium tert- butoxide (ALDRICH, 260 mg, 2.32 mmol) was added and the mixture was stirred at rt for 1 day. The solvent was removed under reduced pressure and the crude was purified by preparative HPLC (SUNFIRE 30x150mm, ACN:H2O 0.1%TFA, gradient 10%-100%) to yield the title compound. 1H NMR (300 MHz, DMSO-d6, 8O0C) delta ppm: 10.70 (s, 1 H), 8.27 (s, 1 H), 7.52-7.38 (m, 3H), 7.23 (d, 1 H), 5.54 (br, 1 H), 3.78 (s, 3H), 3.31 (br., 4H), 2.84 (s, 3H), 2.02-1.78 (m, 4H), 1.74-1.52 (m, 4H). [ES+ MS] m/z 460 (MH)+, 215309-01-6

The synthetic route of 215309-01-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; GLAXO GROUP LIMITED; WO2008/107368; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics