Month: June 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Example 13 N-[6-(4-Allyl-3-methylpiperazin-1-yl)pyridin-3-yl]-4-isopropylbenzenesulfonamide hydrochloride 13.1 3-Methyl-1-(5-nitropyridin-2-yl)piperazine 872 mg (6.31 mmol) of potassium carbonate were added to a solution of 500 mg (3.15 mmol) of 2-chloro-5-nitropyridine in 7 ml of dimethylformamide. After that, a solution of 350 mg (3.32 mmol) of 2-methylpiperazine in 3 ml of dimethylformamide was slowly added dropwise to the reaction mixture while cooling with ice (exothermic reaction). The reaction mixture was stirred for 1 hour while cooling with ice and then stirred overnight at room temperature. After the solvent had been evaporated to dryness, the residue was taken up in water and this mixture was extracted three times with diethyl ether. The combined organic phases were dried over sodium sulfate, filtered and evaporated to dryness, with 3-methyl-1-(5-nitropyridin-2-yl)piperazine (Yield: 650 mg, 89% of theory) being obtained. 1H-NMR (500 MHz, CDCl3): delta [ppm] 9.0 (s, 1H); 8.2 (d, 1H); 6.6 (d, 1H), 4.4 (m, 2H); 3.2 (m, 1H); 3.1 (m, 1H); 2.9 (m, 2H); 2.7 (m, 1H); 1.2 (m, 3H). 13C-NMR (125 MHz, CDCl3): 160.4 (C); 146.5 (CH); 134.9 (C); 133.0 (C); 104.5 (CH); 52.2 (CH2); 50.6 (CH); 45.7 (CH2); 45.4 (CH2); 19.6 (CH3).

109-07-9, 109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Abbott GmbH & Co. KG.; US2006/160809; (2006); 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.122833-04-9,2-Methoxy-4-(4-methylpiperazin-1-yl)aniline,as a common compound, the synthetic route is as follows.,122833-04-9

A solution of the product of EXAMPLE 1F (500 mg, 1.40 mmol), 2-methoxy-4-(4-methylpiperazin-1-yl)aniline (321 mg, 1.68 mmol) and p-toluenesulfonic acid (20 mg, cat.) in n-butanol (10 mL) was heated at 100 C. for 18 hours. After cooling, the mixture was poured into saturated aqueous sodium bicarbonate (100 mL) and the solution was extracted with ethyl acetate (3*50 mL). The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography on silica gel (200-300 mesh) eluting with 20/1 dichloromethane/methanol to afford the title compound. MS: 272.2 (M/2+H+).

The synthetic route of 122833-04-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ABBVIE INC.; Vasudevan, Anil; Penning, Thomas Dale; Chen, Huanming; Liang, Bo; Wang, Shaohui; Zhao, Zhongqiang; Chai, Dikun; Yang, Leifu; Gao, Yingxiang; Pliushchev, Marina; US2014/171429; (2014); 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

A mixture of (R)-tert-butyl-3-(hydroxymethyl)piperazine-1-carboxylate (1 g, 4.62 mmol) and imidazole (0.629 g, 9.24 mmol) was dissolved in CH2Cl2 (10 mL). Tert-butylchlorodiphenylsilane (1.18 mL, 5.08 mmol) was added dropwise over 10 minutes. Upon completion of addition, the mixture was stirred at RT for 3 hours. The reaction mixture was diluted with 50 mL of CH2Cl2 and washed with saturated aqueous sodium bicarbonate (3×20 mL), brine (2×20 mL), dried over magnesium sulfate, and concentrated. Purification via silica gel chromatography using 2-10% methanol in CH2Cl2 gave (R)-tert-butyl-3-(O-tert-butyldiphenylsilane)methyl-piperazine-1-carboxylate as a white solid (1.7 g, 81%). 1H NMR (400 MHz, DMSO-d6) delta 7.63-7.61 (m, 5H), 7.48-7.45 (m, 5H), 4.13-3.44 (m, 5H), 2.80 (d, J=11.8 Hz, 2H), 2.66 (d, J=5.7 Hz, 2H), 1.40 (s, 9H), 1.01 (s, 9H). LC/MS (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)), m/z: M+1 obs=455.5; tR=3.05 min.

278788-66-2, The synthetic route of 278788-66-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Martinborough, Esther; Fanning, Lev T.D.; Sheth, Urvi; Wilson, Dean; Termin, Andreas; Neubert, Timothy; Zimmermann, Nicole; Knoll, Tara; Whitney, Tara; Kawatkar, Arati; Lehsten, Danielle; Stamos, Dean; Zhou, Jinglan; Arumugam, Vijayalaksmi; Gutierrez, Corey; US2008/27067; (2008); 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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Example 28 2-(Phenoxy)ethyl 3-(3-methyl-1-piperazinyl)-2-pyrazinyl Ether The title compound was prepared according to the procedure described in Example 4, Step 2, starting from 2-chloro-3-(2-phenoxyethoxy)pyrazine (150 mg, 0.54 mmol; from Example 1, Step 1) and 2-methylpiperazine (250 mg, 2.5 mmol) with the exception that a final extraction step between EtOAc and 5% aqueous NaOH was carried out. This gave 138 mg (73%) of the title product. Anal. (C17H22N4O2) C, H, N. *Prepared according to the procedure described in Example 4, Step 1., 109-07-9

As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

Reference：
Patent; Biovitrum AB; US6465467; (2002); 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.59702-31-7,1-Ethylpiperazine-2,3-dione,as a common compound, the synthetic route is as follows.,59702-31-7

(2)–To a suspension of 0.71 g of the abovementioned 1-ethyl-2,3-dioxo-piperazine in 15 ml of anhydrous dioxane were added with stirring 0.70 g of trimethylsilyl chloride and 0.83 ml of triethylamine. The resulting mixture was stirred at room temperature for 20 hours to deposit triethylamine hydrochloride. This hydrochloride was separated by filtration, and the filtrate was dropped at 5 to 10 C. into a solution of 0.70 g of phosgene in 10 ml of anhydrous tetrahydrofuran. Subsequently, the resulting mixture was reacted at 5 to 10 C. for 30 minutes and at room temperature for 2 hours, and then the solvent was removed by distillation under reduced pressure to obtain 1.0 g of pale yellow crystals of 4-ethyl-2,3-dioxo-1-piperazinocarbonyl chloride. IR (KBr) cm-1: — nuC=O 1780, 1660

59702-31-7 1-Ethylpiperazine-2,3-dione 108812, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Toyama Chemical Co., Ltd.; US4112090; (1978); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

934-98-5, General procedure: A mixture of celastrol (45mg, 0.1mmol), BOP (53mg, 0.12mmol), DIEA (53muL, 0.3mmol) and 2-dimethylaminoethylamine (28muL, 0.3mmol) in DCM (5.0mL) was stirred at room temperature overnight. Then the mixture was concentrated and purified by normal phase column chromatography (DCM/MeOH=30:1) to afford the target compound as a red solid (35mg, 75.6percent).

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

Reference：
Article; Jiang, Fen; Wang, Hui-Jie; Bao, Qi-Chao; Wang, Lei; Jin, Yu-Hui; Zhang, Qiong; Jiang, Di; You, Qi-Dong; Xu, Xiao-Li; Bioorganic and Medicinal Chemistry; vol. 24; 21; (2016); p. 5431 – 5439;,
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.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

To a stirring solution of piperazin-2-one 16 (500 mg, 5.00 mmol) in CH2C12 (5 mL) under argon atmosphere were added triethylamine (1.5 mL, 10.00 mmol) and Boc- anhydride (1.3 mL, 6.00 mmol) at 0 C; warmed to RT and stirred for 18 h. The reaction was monitored by TLC; after completion of the reaction, the volatiles were removed in vacuo. The crude was purified through silica gel flash column chromatography using 2% MeOH/ CH2C12 to afford compound 17 (450 mg, 45%) as pale yellow solid. TLC: 10% MeOH/ CH2C12 (R/. 0.6); 1H-NMR (DMSO-i/tf, 400 MHz): delta 8.02 (br s, IH), 3.81 (s, 2H), 3.48-3.45 (m, 2H), 3.19-3.14 (m, 2H), 1.41 (s, 9H)., 5625-67-2

As the paragraph descriping shows that 5625-67-2 is playing an increasingly important role.

Reference：
Patent; INDIANA UNIVERSITY RESEARCH AND TECHNOLOGY CORPORATION; ARNOLD, Lee Daniel; MAAG, Hans; TURNER, JR., William W.; (274 pag.)WO2016/168619; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

20327-23-5, 1-Cyclopropylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of N-(l-(lH-indol-3-yl)hexan-2-yl)-2-bromothiazole-5- carboxamide (0.20 g, 0.49 mmol) and 1-cyclopropylpiperazine (0.07 g, 0.54 mmol) in CH3CN (4.5 mL) was added K2CO3 (0.20 g, 1.47 mmol) and the reaction mixture was heated at 80 C for 16 h. The reaction mixture was concentrated in vacuo. The residue was diluted with H20 (10 mL) and extracted with 10% MeOH in DCM (10 mL). The organic layer was separated, dried over anhydrous Na2S04 and concentrated in vacuo. The crude obtained was purified by column chromatography (silica 230-400 mesh, 0 to 10% MeOH in DCM) and then triturating with petroleum ether (6 mL), pentane (10 mL) and DCM (2 mL) to afford N-(l-(lH-indol-3- yl)hexan-2-yl)-2-(4-cyclopropylpiperazin-l-yl)thiazole-5-carboxamide (0.14 g, 63%) as an off- white solid. HPLC Purity: 99.0%. LC/MS (ESI) m/e [M+H]+/RT (min)/%: (0271) 452.00/2.91/98.8%. 1H NMR (400 MHz, DMSO- 6) delta 0.35-0.44 (m, 4H), 0.82 (t, = 6.9 Hz, 3H), 1.16-1.37 (m, 4H), 1.40-1.60 (m, 2H), 1.62-1.68 (m, 1H), 2.60-2.68 (m, 4H), 2.73-2.98 (m, 2H), 3.40-3.48 (m, 4H), 4.04-4.18 (m, 1H), 6.92-6.99 (m, 1H), 7.04 (t, = 7.6 Hz, 1H), 7.09 (s, 1H), 7.31 (d, = 8.3 Hz, 1H), 7.57 (d, = 7.8 Hz, 1H), 7.80 (s, 1H), 7.94 (d, = 8.8 Hz, 1H), 10.75 (brs, 1H).

20327-23-5, 20327-23-5 1-Cyclopropylpiperazine 4742004, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; NEUROPORE THERAPIES, INC.; WRASIDLO, Wolfgang; STOCKING, Emily, M.; HALL, Adrian; MACCOSS, Malcolm; (139 pag.)WO2017/20010; (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.262368-30-9,N-(4-Aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide,as a common compound, the synthetic route is as follows.

130 g of compound C and 89.9 g of material D were added to the reaction flaskCounted as the molar ratio to match the delivery ratio,Compound C was purified) and 1.8 L of methanol,Under the protection of nitrogen, the temperature was stirred to reflux, 1.5-2h after the reaction solution was dissolved, stirring 9-10h, the sample solution for TLC, no compound C was observed, slightly cool to the reaction system by adding 22g25% aqueous ammonia (mass percentage), continue to warm up to reflux for 2h, there is a clear yellow particles solid precipitation, every 2h sampling for HPLC, detected to the compound E residue of less than 0.1%; the end of the reaction slow mixing speed to room temperature (15-20 ), Filtered, 1.2L of water to wash the filter cake, fully dried to dry the dark yellow powder solid, 60 C blast dry to give compound F 170.5g dark brown powder. The molar yield of the Nidanibu free base (Compound F) was 89%, the purity was 99.8%, and the maximum single impurity was less than 0.1%.

262368-30-9, As the paragraph descriping shows that 262368-30-9 is playing an increasingly important role.

Reference：
Patent; Changzhou Jiade Pharmaceutical Technology Co., Ltd.; Wang Zifu; (7 pag.)CN107011241; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

848482-93-9, (S)-4-(tert-Butoxycarbonyl)piperazine-2-carboxylic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

848482-93-9, To a stirred solution of (S)-4-(tert-butoxycarbonyl)piperazine-2-carboxylic acid (CAS Number 848482-93-9; 0.540 g, 2.35 mmol) in MeOH (15 ml) was added 37% aqueous formaldehyde solution (0.2 ml) and a catalytic amount of acetic acid, followed by 10% dry Pd/C (0.100 g) under nitrogen atmosphere at rt. The reaction mixture was purged with H2 gas at rt for 2 h. The resulting reaction mixture was carefully filtered through celite hyflow and the filtrate was concentrated under reduced pressure. The residue was triturated with n-pentane (5 ml) to obtain a solid material, which was dried under high vacuum to yield (S)-4-(tert-butoxycarbonyl)-1 – methylpiperazine-2-carboxylic acid (0.300 g, 1 .23 mmol). This material was used directly for the next step without further purification. LCMS: Method C, 1 .560 min, MS: ES+ 245.33.

848482-93-9 (S)-4-(tert-Butoxycarbonyl)piperazine-2-carboxylic acid 1501850, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; MISSION THERAPEUTICS LIMITED; STOCKLEY, Martin Lee; KEMP, Mark Ian; MADIN, Andrew; (167 pag.)WO2018/65768; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics