Tag: M.W:100-200

5308-25-8, 1-Ethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5308-25-8, 1-(Bromomethyl)-4-nitro-2-(trifluoromethyl)benzene (34 g, 120 mmol) obtained in Step (1) above was stirred in a solvent of dichloromethane (300 mL). The reaction solution was added with 1-ethylpiperazine (15.97 mL, 126 mmol) and DIPEA (27.2 mL, 156 mmol), followed by stirring for about 3 hours at room temperature. The reaction mixture was diluted with dichloromethane, washed with a saturated aqueous sodium bicarbonate solution and saline. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain the title compound (21.7 g, 57%). 1H-NMR Spectrum (300 MHz, DMSO-d6): delta 8.52 (d, 1H), 8.40 (s, 1H), 8.09 (d, 1H), 3.71 (s, 2H), 2.35 (m, 10H), 1.00 (t, 3H). MS (ESI+, m/z): 318 [M+H]+

As the paragraph descriping shows that 5308-25-8 is playing an increasingly important role.

Reference：
Patent; HANMI PHARM. CO., LTD.; Bae, In Hwan; Han, Sang Mi; Kwak, Eun Joo; Ahn, Young Gil; Suh, Kwee Hyun; US2015/191450; (2015); 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.75336-86-6,(R)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

75336-86-6, To the 1200 L reactor was dissolved (R)-2-methylpiperazine from Example 5 (25 kg) in CH3CN (319 kg) at [15°C] to [25°C] until dissolution was complete (10 min. ) After cooling to [5°C] to [10°C] Et3N (63 kg) was added. To the 1200 L receiver trityl chloride (69.5 kg) was dissolved in CH2C12 (106 kg) at [15°C] to [25°C.] The solution in the receiver was transferred to the reactor over 0.5 h with a CH2C12 rinse (27 kg), and the solution was heated to [20°C] to [30°C.] The reaction was monitored by GLC and was complete in 1 h. The resulting slurry was cooled to [8°C] to [12°C,] filtered onto a 48″Nutsche filter, and rinsed with CH3CN (40 kg at [8°C] to [12°C).] The filter cake was dried using [50°C] to [55°C] nitrogen to afford 25.26 kg of the by-product [ET3NHCL] (74percent yield; easy to filter off the by-product). The filtrate was transferred to the 1200 L reactor and cooled further [TO-8°C] [TO-10°C] for 1 h. The resulting slurry was filtered onto a 24″Nutsche filter and rinsed [WITH-8°C] to-10°C CH3CN (24 kg) sending the filtrate and rinse to the 1200 L receiver. The filter cake was dried with [50°C] to [55°C] nitrogen to afford another 2.98 kg [ET3NHCL] (9percent yield). The filtrate was transferred to the 1200 L reactor with a CH3CN (10 kg) rinse, and distilled under vacuum to an oil of the title compound of 97.99percent GC purity. The yield was quantitative. M. Pt. [134-136°C.] [APOS;H] NMR (400 MHz, CDC13) : [6] 7.55-7. 40 (6H, br s), 7.25 (6H, t, J = 7. 9 Hz), 7.14 (3H, t, [J =] 7.1 Hz), 3.21-3. 13 (2H, [M),] 3. [10-2. 90 (1H,] br s), 2.94 (2H, t, J = 13.0 Hz), 1.60 [(1H,] br s), 1.48 (1H, br s), 1.15 (1H, br s), 0.94 (3H, d, J = 6.1 Hz), 0.00 (TMS, reference). [13C] NMR (100 MHz, CDC13) : [6] 129.41 (d), 127.46 (d), 125.96 (d), 125.83 (s), 56.12 (t), 51.23 (d), 48.73 (t), 46.45 (t), 20.05 (q), 0.00 (TMS, reference). IR (diffuse reflectance) 2964,2835, 2483 (w), 2350 (w), 2339 (w), 1956 (w), 1490,1025, 909,742 (s), 717,710 (s), 703 (s), 697 (s), 629, [CM-1.] HRMS [(EI)] calcd for [C24H26N2] 342.2096, found [342. 2101.] [a] [25D=-12° (C 1. 00, CH2CL2).] Anal. Calcd for [C24H26N2] : C, 84.17 ; H, 7.65 ; N, 8.18. Found: C, 84.12 ; H, 7.64 ; N, 7.94.

75336-86-6 (R)-2-Methylpiperazine 7330434, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; BIOVITRUM AB; WO2004/829; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, PPh3 (0.0325 mol) was added dropwise at a temperature between 0 and [5°C] to a solution of Vanillin (CA No : [121-33-5)] (0. [025 MOL),] intermediate 14 (0.03 mol) and DIAD (0.0375 mol) in THF (60ml). The mixture was stirred at room temperature for 18 hours. EtOAc was added. The mixture was extracted twice with [HC13N.] The acidic layer was washed with EtOAc, basified with [K,, C03] and extracted with EtOAc. The organic layer was dried [(MGS04),] filtered, and the solvent was evaporated. Yielding: 3.9g of intermediate 15 [(56percent).

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference：
Patent; JANSSEN PHARMACEUTICA N.V.; WO2004/7498; (2004); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

59702-07-7, EXAMPLE 18 4-Methyl-3-oxo-piperazine-1-carboxylic Acid (4-methoxy-7-piperidin-1-yl-benzothiazol-2-yl)-amide Using 4-methoxy-7-piperidin-1-yl-benzothiazol-2-ylamine and 4-methyl-3-oxo-piperazine, the title compound was prepared as yellow solid in 84percent yield. MS: m/e=404(M+H+).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Flohr, Alexander; Jakob-Roetne, Roland; Norcross, Roger D.; Riemer, Claus; US2003/149036; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

25057-77-6, 1,2-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Reference Example 7 To a solution of N-benzyl-4-piperidone (8.0 g) and 3,4-dimethylpiperazine (9.5 g) in ethanol (100 ml) are added 5% platinum-carbon (2 g) and acetic acid (14.4 ml), and the mixture is subjected to catalytic hydrogenation at room temperature under atmospheric pressure. The catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure. Water is added to the resultant, and the mixture is basified with a 5% aqueous sodium hydroxide solution, and the mixture is extracted with diethyl ether. The extract is washed with water, dried and concentrated under reduced pressure to remove the solvent. The residue is dissolved in ethanol, and thereto is added to conc. hydrochloric acid to give a hydrochloride. The resulting white powder is collected by filtration, dissolved in water, and basified with a 5% aqueous sodium hydroxide solution. The mixture is extracted with diethyl ether, washed with water, dried, and concentrated under reduced pressure to give 4-(3,4-dimethyl-1-piperazinyl)-1-benzylpiperidine (4.2 g). 1 H-NMR (CDCl3) deltappm: 1.04 (3H, d, J=6 Hz), 1.45-2.5 (12H, m), 2.27 (3H, s), 2.7-3.05 (4H, m), 3.48 (2H, s), 7.31 (5H, m).

25057-77-6, The synthetic route of 25057-77-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Otsuka Pharmaceutical Company, Limited; US6140330; (2000); 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.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.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.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

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.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