Month: September 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.59878-57-8,1-(Cyclopropylcarbonyl)piperazine,as a common compound, the synthetic route is as follows.,59878-57-8

3-((4-oxo-3,4-dihydro-phthalazin-1-yl-oxyl) benzoic acid (54 mg, 0.3 mmol) was dissolved in N, N-dimethylformamide, and then 1-(3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDCI) (220 mg, 1.2 mmol), triethylamine(150 muL, 1.2 mmol) and 1-hydroxy-7-azabenzotriazole (HOAt)(165 mg, 1.2 mmol) were added successively. The mixture was stirred at room temperature for half an hour, and then N-(cyclopropanecarbonyl) piperazine was added and reacted at room temperature overnight, and then the reaction was quenched with water, extracted with ethyl acetate, and washed with water for three times. The organic phases were combined and washed with saturated saline, dried with anhydrous sodium sulfate, and concentrated for column chromatography isolation (dichloromethane:methanol=20:1) to give Compound 7. A white solid was obtained. 1H NMR (600 MHz, DMSO-d6): delta 11.98 (s, 1H), 8.27 (d, 1H, J = 7.38 Hz), 8.10 (d, 1H, J = 7.74 Hz), 7.99-8.01 (m, 1H), 7.94-7.96 (m, 1H), 7.52 (t, 1H, J= 7.86 Hz), 7.39-7.38 (m, 2H), 7.28 (d, 1H, J = 7.62 Hz), 3.33-3.81 (m, 8H), 1.96 (brs, 1H), 0.69-0.74 (m, 4H); ESI-MSm/z: calculated for 418.16, found 417.89 [M-H]+.

59878-57-8 1-(Cyclopropylcarbonyl)piperazine 2064235, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Chengdu Di’ao Pharmaceutical Group Co. Ltd.; JI, Jianxin; GUO, Na; XUE, Ting; KANG, Bingqiang; YE, Xinfa; CHEN, Xin; ZHANG, Tao; EP2799435; (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.219509-79-2,1-tert-Butyl 4-methyl piperazine-1,4-dicarboxylate,as a common compound, the synthetic route is as follows.

The compound 1-tert-butoxycarbonyl-2,4-piperazine carboxylate (0.18g, 0.61mmol) in dichloromethane(6mL) was added HCl in ethyl acetate solution (4M, 3mL), stirred at rt for 1h, the solvent was removed to give awhite solid 146mg: 1,3-piperazine compound Two carboxylate hydrochloride, yield: 99%., 219509-79-2

219509-79-2 1-tert-Butyl 4-methyl piperazine-1,4-dicarboxylate 11118267, 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

109384-27-2, 1-Methylpiperazin-2-one hydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 51A 6-chloro-2-methyl-5-(4-methyl-3-oxopiperazin-1-yl)pyridazin-3(2H)-one [0791] A mixture of Example 18B (0.179 g, 1.0 mmol), 1-methylpiperazin-2-one, hydrochloric acid (0.301 g, 2 mmol), and triethylamine (0.405 g 4.0 mmol) in ethanol (10 mL) was heated under reflux for 16 hours. The solvent was removed, and the residue was purified by flash column chromatography on silica gel eluting with 1-5% methanol in ethyl acetate to afford 0.21 g (82%) of the title compound.

109384-27-2, As the paragraph descriping shows that 109384-27-2 is playing an increasingly important role.

Reference：
Patent; HUBBARD, Robert D.; WANG, Le; PARK, Chang H.; SUN, Chaohong; McDANIEL, Keith F.; PRATT, John K.; SOLTWEDEL, Todd N.; WENDT, Michael D.; HOLMS, John H.; LIU, Dachun; SHEPPARD, George S.; US2013/331382; (2013); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-01-3

A mixture of 3-bromopropanol (20 ml), N-methylpiperazine (29 ml), potassium carbonate (83 g) and ethanol (200 ml)was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2.8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H).

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; AstraZeneca AB; US2004/48881; (2004); A1;; ; Patent; Lambert, Christine Marie Paul; Ple, Patrick; US2004/44015; (2004); 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.13484-40-7,1-(2-Methoxyethyl)piperazine,as a common compound, the synthetic route is as follows.

A solution of (i?)-3-(6-(2- fluorophenyl)-5,6-dihydrobenzo[h]quinazolin-2-ylamino)phenethyl methanesulfonate (5.37 g, 11.00 mmol), l-(2-methoxyethyl)piperazine (3.32 niL, 22.34 mmol) and triethylamine (1.5 niL, 11.17 mmol) in JV,JV-dimethylacetamide (30 mL) was heated at 90 0C for 20 h. After cooling to room temperature, water (200 mL) was added while stirring. The suspension was stirred for 15 min. and filtered. Solid was taken into dichloromethane (200 mL), dried over sodium sulfate and concentrated. Product was purified by flash column chromatography on silica gel (120 g silica gel column, 0-10% 7N NH3 in methanol-dichloromethane, over 80 min.) to afford the title compound as a yellow solid (5.50 g, 93% yield). 1H-NMR (DMSO- d6): delta 9.53 (s, 1 H), 8.37-8.34 (m, 1 H), 8.33 (s, 1 H), 7.81 (s, 1 H), 7.62-7.60 (m, 1 H), 7.51- 7.46 (m, 2 H), 7.30-7.19 (m, 3 H), 7.08-7.02 (m, 2 H), 6.82-6.79 (m, 2 H), 4.67 (t, J= 7.2 Hz, 1 H), 3.41 (t, J= 5.6 Hz, 2 H), 3.22-3.08 (m, 2 H), 3.33 (s, 3 H), 2.74-2.70 (m, 2 H), 2.59- 2.42 (m, 12 H). LCMS m/e 539 [M+H].

13484-40-7, As the paragraph descriping shows that 13484-40-7 is playing an increasingly important role.

Reference：
Patent; ARQULE, INC.; ALI, Syed, M.; ASHWELL, Mark; TANDON, Manish; YANG, Rui-yang; LIU, Yanbin; VENSEL, David; EATHIRAJ, Sudharshan; PALMA, Rocio; LAPIERRE, Jean-marc; WESTLUND, Neil; WU, Hui; NAMDEV, Nivedita; KELLEHER, Eoin; KELLEHER, Eugene; WO2010/78421; (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.314741-40-7,(S)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

A solution of iert-butyldimethylsilyl chloride (1.53 g, 10.17 mmol) in DCM (10 ml) was added dropwise to (5)-4-A/-Boc-2-hydroxymethyl-piperazine (2 g, 9.25 mmol) and triethylamine (2.58 ml, 18.49 mmol) in DCM (50 ml) at 20C over a period of 5 minutes under air. The resulting solution was stirred at 20C for 16 hours then evaporated to dryness. The residue was purified by flash silica chromatography, elution gradient 0 to 5% EtOH in EtOAc. Pure fractions were evaporated to dryness to afford te/t-butyl (S)-3-(((ieri-butyldimethylsilyl)oxy)methyl)piperazine-l-carboxylate (2.84 g, 93%) as a colourless oil. 1H NM (500 MHz, CDCI3) 0.00 (s, 6H), 0.84 (s, 9H), 1.40 (s, 9H), 2.48 (s, 1H), 2.6 – 2.87 (m, 3H), 2.92 (d, J = 11.5 Hz, 1H), 3.41 (dd, J = 7.2, 9.8 Hz, 1H), 3.52 (s, 1H), 3.85 (s, 2H).

314741-40-7, The synthetic route of 314741-40-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; KETTLE, Jason, Grant; BAGAL, Sharanjeet, Kaur; BOYD, Scott; EATHERTON, Andrew, John; FILLERY, Shaun, Michael; ROBB, Graeme, Richard; RAUBO, Piotr, Antoni; (144 pag.)WO2018/206539; (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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 4 Sodium hydride (50% dispersion in mineral oil) (0.8 g.) is added to a suspension of 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (4.63 g.) in anhydrous dimethylformamide (45 cc.), whilst keeping the temperature between 18-20 C. The reaction mixture is stirred for a further 4 hours 30 minutes. A solution of 1-chlorocarbonyl-4-methylpiperazine (2.7 g.) in anhydrous dimethylformamide (25 cc.) is then added over the course of 15 minutes and at a temperature of 20 C. The suspension is stirred for 17 hours at a temperature of about 20 C., and then anhydrous hexamethylphosphotriamide (7 cc.) is added. After 15 minutes, the reaction mixture is poured into ice-water (500 g.). The precipitate is filtered off and washed with water (45 cc.). A product (6.1 g.) is obtained and is recrystallized from diisopropyl ether (1,500 cc.). 2-(7-Methoxy-1,8 -naphthyridin-2-yl)-3-(4-methylpiperazin-1-yl)carbonyloxy-isoindolin-1-one (3 g.), melting at 191 C., is thus obtained. The 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one can be prepared in the following way: Preparation of 2-acetylamino-7-chloro-1,8-naphthyridine, m.p. 251-253 C., according to S.

39539-66-7, 39539-66-7 4-Methylpiperazine-1-carbonyl chloride 3016935, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); 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.76003-30-0,1-Boc-2-methyl-3-oxopiperazine,as a common compound, the synthetic route is as follows.

76003-30-0, To a heterogeneous mixture of Lawesson’s reagent (2.11 g, 5.06 mmol) in toluene (18 mL) was added the product of Example 1, step a (1.01 g, 4.73 mmol). The mixture was heated at 80 C for 1 h and then concentrated in vacuo. The residue was dissolved in DCM and filter loaded on Si02 column eluting with EtO Ac/Hex to afford the desired product as an orange solid (1.12 g, 100%).

The synthetic route of 76003-30-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; JANSSEN PHARMACEUTICA NV; ANDRES GIL, JOSE IGNACIO; LETAVIC, MICHAEL A; RECH, JASON C; RUDOLPH, DALE A; SOYODE-JOHNSON, AKINOLA; CHROVIAN, CHRISTA C; (158 pag.)JP2017/527588; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

129779-30-2, (3R,5S)-rel-tert-Butyl 3,5-dimethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 1,3-dibromobenzene (1.10 g, 4.67 mmol), (cis)-tert-butyl 3,5- dimethylpiperazine- 1 -carboxylate (0.5 g, 2.33 mmol) and 2-dicyclohexylphosphino-2?,6?- dimethoxy- 1,1 ?-biphenyl (47.9 mg, 0.117 mmol) in THF (15 mL) in a pressure reactionvial was purged with nitrogen. Tris(dibenzylideneacetone)dipalladium(0) (42.7 mg,0.047 mmol) was added, followed by lithium bis(trimethylsilyl)amide (7.0 mL, 7.0 mmol,1 N in THF). The mixture was purged with nitrogen for several mm and then capped andheated at 70 C for 2.5 h. The reaction mixture was cooled and quenched with aq.NaHCO3, then diluted with 75 mL of EtOAc, washed with H20, brine, dried andconcentrated. The residue was purified on silica gel, with a linear gradient of 0-100%EtOAc/hexanes to give (cis)-tert-butyl 4-(3 -bromophenyl)-3 ,5 -dimethylpiperazine- 1- carboxylate (0.505 g) as an oil. LCMS, M+H = 369.2/37 1.2 Method G. Rt. 3.55 mm.

129779-30-2, The synthetic route of 129779-30-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; BRISTOL-MYERS SQUIBB COMPANY; BHIDE, Rajeev S.; BATT, Douglas G.; CHERNEY, Robert J.; CORNELIUS, Lyndon A.M.; LIU, Qingjie; MARCOUX, David; NEELS, James; POSS, Michael A.; QIN, Lan-ying; RUAN, Zheming; SHI, Qing; SRIVASTAVA, Anurag S.; TINO, Joseph A.; WATTERSON, Scott Hunter; (532 pag.)WO2016/64957; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

548762-66-9,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.548762-66-9,(2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

(b) (2S,5R)-4-[5-(4-Bromo-3-trifluoromethoxy-phenylcarbamoyl)-pyridin-2-yl]-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester The product of the previous step (3.86 g, 10.2 mmol) (2S,5R)-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (2.62 g, 12.2 mmol) and N,N-diisopropylethylamine (5.32 mL, 30.5) was dissolved in DMSO (12 mL). The reaction mixture heated at 120 C. for 3 h, diluted with EtOAc (100 mL), washed with water, and saturated NH4Cl, water, and brine. The reaction mixture was evaporated to about 40% volume and 3 M HCl in cyclopentyl methyl ether (4.24 mL, 12.7 mmol) was added slowly. Seeds from a previous run at smaller scale were added and the reaction mixture was stirred for 2 days and filtered to provide the HCl salt of the title intermediate (5.15 g, 83% yield). Analytical HPLC: Retention time=21.1 min.

The synthetic route of 548762-66-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Thalladi, Venkat R.; Nzerem, Jerry; Huang, Xiaojun; Zhang, Weijiang; US2013/295048; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics