Month: May 2021

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.,934-98-5

To Example 9P (8.8 g) in a mixture of anhydrous dichloromethane (100 mL) and acetic acid (20 mL) was added 2-(4-methylpiperazin-l-yl)ethanamine (3.16 g). The mixture was stirred at room temperature for 1 hour before sodium triacetoxyborohydride (7.02 g) was added. The reaction mixture was stirred at room temperature overnight. The volatiles were removed by rotary evaporation, and the residue was dissolved in tetrahydrofuran (45 mL) and water (7.5 mL). The mixture was cooled to 0 °C, and trifluoracetic acid (45 mL) was added. After the addition, the cooling bath was removed, and the mixture was stirred at room temperature for 4 hours. The mixture was diluted with ethyl acetate. The mixture was washed with a pre-cooled diluted sodium hydroxide mixture (contained about 60 mL of 50percent sodium hydroxide mixture, pH 10) and brine. The organic phase was concentrated. The intermediate was dissolved in anhydrous dichloromethane (100 mL). Anhydrous magnesium sulfate (25 g) was added. The mixture was stirred at room temperature overnight, and sodium triacetoxyborohydride (7.02 g) was added. The reaction mixture was stirred at room temperature for 4 hours. The material was filtered off, and the filtrate was directly purified by silica gel chromatography (0-20percent methanol containing 3percent ammonium hydroxide in dichloromethane) to provide the title compound. MS (ESI) m/z 850 (M+H)+.

As the paragraph descriping shows that 934-98-5 is playing an increasingly important role.

Reference：
Patent; ABBVIE INC.; ABBVIE DEUTSCHLAND GMBH & CO. KG; BRAJE, Wilfried; DOHERTY, George; JANTOS, Katja; JI, Cheng; JUDD, Andrew; KUNZER, Aaron; MASTRACCHIO, Anthony; SONG, Xiaohong; SOUERS, Andrew; SULLIVAN, Gerard; TAO, Zhi-Fu; LAI, Chunqui; KLING, Andreas; POHLKI, Frauke; TESKE, Jessc; WENDT, Michael; BRADY, Patrick; WANG, Xilu; PENNING, Thomas; MICHAELIDES, Michael; (448 pag.)WO2019/35927; (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.20327-23-5,1-Cyclopropylpiperazine,as a common compound, the synthetic route is as follows.

Example 277 Synthesis of 3-[1-{4-[2-(4-Cyclopropyl-piperazin-1-yl)-2-oxo-ethyl]-3,5-dimethyl-1H-pyrrol-2-yl }-meth-(Z)-ylidene]-5-(2,6-dichloro-phenylmethanesulfonyl)-1,3-dihydro-indol-2-one A mixture of {5-[5-(2,6-dichloro-phenylmethanesulfonyl)-2-oxo-1,2-dihydro-indol-(3Z)-ylidenemethyl]-2,4-dimethyl-1H-pyrrol-3-yl}-acetic acid (208 mg, 0.4 mmol), HOBt (54 mg, 1 eq.) and EDAC (153 mg, 2 eq.) in DMF (1.5 mL) was stirred at rt for 30 mins. To the mixture was added 1-cyclopropyl-piperazine (101 mg, 2 eq.) in DMF (1.5 mL). After stirring at rt for overnight, the precipitate was collected by vacuum filtration, washed with water, sodium bicarbonate and ether to give 108 mg (43%) of the titled compound. 1H-NMR (400 MHz, DMSO-d6) delta 13.46 (s, 1H, NH), 11.26 (s, 1H, NH), 8.17 (d, 1H), 7.76 (s, 1H), 7.48 (d, 1H), 7.46 (s, 1H), 7.36 (m, 2H), 6.99 (d, J=8 Hz, 1H), 4.84 (s, 2H), 3.49 (s, 2H), 3.46 (m, 2H), 3.39 (m, 2H), 2.47 (m, 4H), 2.25 (s, 3H, CH3), 2.22 (s, 3H, CH3), 1.6 (m, 1H), 0.4 (m, 2H), 0.31 (m, 2H). MS m/z 625 [M-1]., 20327-23-5

As the paragraph descriping shows that 20327-23-5 is playing an increasingly important role.

Reference：
Patent; SUGEN, INC.; US2003/125370; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

262368-30-9, N-(4-Aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of methyl (E)-1-acetyl-3-(methoxyphenylmethylene)-oxindole-6-carboxylate of formula 2 (7.03 g), N-(4-aminophenyl)-N,4-dimethyl-1-piperazine acetamide (5.30 g) and methanol (50 ml) was stirred under reflux for 5 h. The bath temperature was reduced to 70C and, at this temperature, a solution of KOH (containing 85% of KOH; 0.13 g) in methanol (2 ml) was added dropwise. The reaction mixture was stirred at 70 to 60C for 30 mm, then itwas left to stand at 20C for 2 h and the crystallization of the product was completed in 2 h at10C. The product was filtered off, washed with glacial methanol twice and air-dried. The yield was 9.71 g (90%) of a yellow powder. HPLC purity 99.86%.

262368-30-9, 262368-30-9 N-(4-Aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide 21927707, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ZENTIVA, K.S.; MECA, Ludek; (16 pag.)WO2017/16530; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

196811-66-2, tert-Butyl 4-carbamothioylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 2-chloro-l-(4,5-dihydro-5-phenyl-3-isoxazolyl)ethanone (i.e. the product of Step C) (0.450 g, 2.018 mmol) and 1,1-dimethylethyl 4-(amino-thioxomethyl)-l- piperazinecarboxylate (i.e. the product of Step A) (0.5 g, 2.04 mmol) in ethanol (10 mL) was added triethylamine (0.204 g, 2.013 mmol), and the reaction mixture was stirred at room temperature for 12 h. The reaction mixture was concentrated under reduced pressure, and the residue was partitioned between ethyl acetate (30 mL) and water (30 mL). The organic layer was separated and washed with brine (25 mL), dried (Na2S04), and concentrated under reduced pressure. The crude residue was purified by column chromatography using 20% ethyl acetate in petroleum ether as eluant to give 700 mg of the title compound as a white solid..H NMR (CDCI3) delta 1.48 (s, 9H), 3.30 (m, 1H), 3.54 (m, 8H), 3.74 (m, 1H), 5.71 (m, 1H), 6.91 (s, 1H), 7.40-7.29 (m, 5H).

196811-66-2, The synthetic route of 196811-66-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; E. I. du Pont de Nemours and Company; DUNG, Mei H.; PASTERIS, Robert, James; WO2011/72207; (2011); 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.129799-15-1,Methyl 1-Boc-piperazine-2-carboxylate,as a common compound, the synthetic route is as follows.

To a solution of N-1-Boc-2-piperazinecarboxylic acid methyl ester (CAS Reg. No: [129799-15-1]) (1 g) in DMF (5 mL) was added 3-chlorobenzenesulfonyl chloride (0.95 g) and triethylamine (1.71 mL). The reaction mixture was stirred at RT overnight. Water was added and the mixture was extracted with ethyl acetate (x2). The combined organic layers were washed with water (×2) and brine, were dried (Na2SO4), filtered and evaporated. Purification by chromatography (SiO2, n-heptane/ethyl acetate 3:1) yielded 4-(3-chloro-benzenesulfonyl)-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester as white foam (1.66 g), MS: 436.3 ([M+NH4, 1Cl]+)., 129799-15-1

The synthetic route of 129799-15-1 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Dehmlow, Henrietta; Kuhn, Bernd; Sander, Ulrike Obst; Roever, Stephan; Schulz-Gasch, Tanja; Wright, Matthew; Wyler, Rene; US2009/48264; (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.120737-78-2,tert-Butyl 2-methylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

To a stirred solution of 3-bromobiphenyl (0.70 g, 3.00 mmol) in toluene (10 mL) was added t-butyl 2-methylpiperazine-l-carboxylate (0.720 g, 3.60 mmol), potassium t- butoxide (0.504 g, 4.50 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.090 g, 98.3 mmol) and tri-t-butylphosphine (0.018 g, 89.0 mmol). The mixture was heated at 90 C for 5 hours. At this time the reaction was cooled, diluted with water and extracted with ethyl acetate. The combined extracts were washed with brine, dried (Na2S04) and concentrated. The residue was purified by flash chromatography over silica using a hexane/ethyl acetate eluant to afford t-butyl 4-([l, -biphenyl]-3-j/j-2-methylpiperazine- 1-carboxylate (0.750 g, 71%) as a brown oil. The t-butoxycarbonyl protecting group was removed from this compound using General Procedure G to afford l-([l,l’-biphenyl]-3- yl)-3-methylpiperazine. This intermediate was, in turn, was reacted with Intermediate 5 using General Procedure A to generate the title compound. 1H NMR (500 MHz, CDCI3) delta 7.60-7.34 (m, 6H), 7.12-7.11 (m, 2H), 6.92-6.90 (m, 1H), 4.40-4.39 (d, J= 6.5 Hz, 1H), 4.19-4.14 (m, 1H), 3.87-3.33 (m, 4H), 3.09-2.88 (m, 8H), 2.46-2.43 (m, 1H), 1.99-1.55 (m, 9H), 1.38 (t, J = 7.0 Hz, 3H) ppm. 13C NMR (125 MHz, CDC13) delta 156.7, 156.7, 151.9, 142.5, 141.6, 129.5, 128.7, 127.3, 127.2, 119.1, 115.4, 115.4, 115.3, 115.3, 59.0, 54.3, 54.3, 53.2, 53.3, 49.1, 49.1, 47.9, 47.8, 47.7, 47.7, 46.1, 46.0, 39.8, 39.5, 39.1, 39.0, 36.7, 36.4, 25.9, 25.8, 25.4, 24.3, 24.3, 24.1, 24.0, 15.8, 15.7 ppm. Purity: >99% (214 & 254 nm) LCMS; retention time: 1.29 min; (M+H+) 433.3

120737-78-2, The synthetic route of 120737-78-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; GENZYME CORPORATION; BOURQUE, Elyse; CABRERA-SALAZAR, Mario, A.; CELATKA, Cassandra; CHENG, Seng, H.; HIRTH, Bradford; GOOD, Andrew; JANCSICS, Katherine; MARSHALL, John; METZ, Markus; SCHEULE, Ronald, K.; SKERLJ, Renato; XIANG, Yibin; ZHAO, Zhong; LEONARD, John; NATOLI, Thomas; MAKINO, Elina; HUSSON, Herve; BESKROVNAYA, Oxana; WO2014/43068; (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.57260-70-5,tert-Butyl 4-benzylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Compound lOA was treated with 30 mL EA solution of HCl (1 M) and stirred at rt for18.5 hrs. The mixture was concentrated in vacuo to give about 135 mg of 1-benzylpiperazine(Compound lOB) as a white solid which was used directly in the next step. MS: calc’d 177(M+Ht, measured 177 (M+Ht.

57260-70-5, The synthetic route of 57260-70-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; WANG, Lisha; YUN, Hongying; ZHANG, Weixing; ZHU, Wei; ZHANG, Zhiwei; (69 pag.)WO2017/202704; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

30459-17-7, 1-(4-Trifluoromethylphenyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: The mixture of intermediate 2 (267 mg, 1.0 mmol), co-responding amines and Zn(ClO4)2. 6H2O (7.4 mg, 2.0 mol %) in dichloromethane (5 mL) was stirred at room temperature under argon. After completion of the reaction, the mixture was diluted with water and extracted with dichloromethane(3×30 mL). The combined dichloromethane was dried over anhydrous sodium sulfate and solvent was removed under reduced pressure to give target compounds 6a-n (Table 2) which were purified by column chromatography eluting with chloroform : methanol., 30459-17-7

30459-17-7 1-(4-Trifluoromethylphenyl)piperazine 121718, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Van Chinh, Luu; Anh, Le Duc; Nga, Nguyen Thi; Ly, Nguyen Thi Hai; Ha, Vu Thi; Toan, Tran Quoc; Cuong, Nguyen Manh; Vu, Tran Khac; Letters in Organic Chemistry; vol. 14; 8; (2017); p. 603 – 611;,
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.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 11; Synthesis of Active Esters Of N-Methyl Piperazine Acetic Acid Via Oxalyl Chloride (Scheme B, FIG. 4B); To a suspension of N-methyl piperazine acetic acid (N-MPAA) (79 mg, 0.5 mmol) in DCM (25 mL) was added a solution of oxalyl chloride (4 mL, 0.8 mmol, 2.0 M solution in DCM) over 10 minute at room temperature. After another 30 minutes of reaction, solvent and excess reagent were removed under reduced pressure to give a white solid (23). A solution of NHS (57 mg, 0.5 mmol) in DCM (25 mL) was added to the solid followed by ss-TBD (390 mg, 1 mmol, 2.6 mmol/g). The resulting solution was sonicated for 5 minute when all solid dissolved. The ss-TBD resin was removed by filtration and solvent was evaporated to yield a white foam (97% yield). Product was characterized by ES-MS as before.

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

183742-34-9, 4-Boc-1-Fmoc-2-piperazineacetic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 2-(l-(((9Eta-fluoren-9-yl)methoxy)carbonyl)-4-(ter?- butoxycarbonyl)piperazin-2-yl)acetic acid (5 g, 10.72 mmol) in dichloromethane (100 mL) with Lambda/,Lambda/-dimethylformamide (2 drops) was added oxalyl dichloride (3.4 g, 26.8 mmol). The reaction mixture was stirred at room temperature for 1 hour, then concentrated. Tetrahydrofuran (100 mL) was added to the concentrate followed by the slow addition of a solution containing 2-bromo-6-fluoroanaline (3 g, 16 mmol) and diisopropylethylamine (9 mL) in tetrahydrofuran (20 mL). The solution was stirred at room temperature for 2 hours before the addition of piperazine (2.77 g, 32.2 mmol) after which the solution was stirred for 15 hours. The reaction mixture was concentrated onto silica gel and purified via flash chromatography (0-100 % ethyl acetate/hexane, then 0-10 % methanol/dichloromethane) to afford the title compound. 1H NMR (300 MHz, DMSO-J6) delta ppm 7.47 – 7.65 (m, 1 H) 7.21 – 7.46 (m, 2 H) 3.55 – 4.05 (m, 2 H) 2.67 – 3.14 (m, 3 H) 2.49 – 2.67 (m, 2 H) 2.26 – 2.46 (m, 2 H) 1.39 (s, 9 H); MS (APCI+) m/z 418.2 (M+H)+.

183742-34-9, As the paragraph descriping shows that 183742-34-9 is playing an increasingly important role.

Reference：
Patent; ABBOTT LABORATORIES; ABBOTT GMBH &; CO. KG; WANG, Ying; BREWER, Jason, T.; AKRITOPOULOU-ZANZE, Irini; DJURIC, Stevan, W.; POHLKI, Frauke; BRAJE, Wilfried; RELO, Ana-Lucia; WO2010/124042; (2010); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics