Month: January 2021

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

General procedure: A solution of 4-fluoronitrobenzene 6 (2 g, 14.2 mmol) and anhydrous K2CO3 (2.2 g, 15.6 mmol) in DMSO (5 mL) was stirred at room temperature for 10 min. The appropriate secondary amine (14.2 mmol) was added dropwise, and the resulting reaction mixture was stirred at room temperature for 10 h. The mixture was then poured into ice-water to form a precipitate collected by filtration then dried to give the nitrophenyl derivative 7a-7e.

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

Reference£º
Article; Elkamhawy, Ahmed; Al-Sanea, Mohammad M.; Song, Chiman; Sim, Taebo; Roh, Eun Joo; Bulletin of the Korean Chemical Society; vol. 36; 7; (2015); p. 1863 – 1873;,
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.

To a 0 0C cooled solution of 4-nitrobenzaldehyde in DCM (40 mL) was added Na(OAc)3BH (10.526gm, 49.66 mmol) and the reacton was stirred for lOmin. To the reaction mixture was added N-methylpiperazine (9.93 g, 99.3 mmol) under nitrogen atmosphere and the reaction mixture was continued stirring at room temperature for 4h. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was partitioned between DCM (20 mL) and water (15 mL) and the organic layer was separated, washed with water (2 x 15 mL), dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave l-methyl-4-(4-nitrobenzyl)piperazine (4 g). 1H NMR (CDCl3, 200MHz) delta: 8.19 (2H, d, J= 8.4Hz), 7.53 (2H5 d, J= 8.4 Hz)5 3.59 (2H, s), 2.47 (8H, bm), 2.29 (3H5 s); m/e = 236 (M+l). To a solution of l-methyl-4-(4-nitrobenzyl)piperazine (4.0 g) in methanol (100 niL) at room temperature under nitrogen atmosphere was added Raney nickel (1.6gm). The reaction mixture was stirred for 2 hr under hydrogen atmosphere. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was filtered under nitrogen atmosphere and the solvent was removed under reduced pressure to give 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g). 1H NMR (CDCl3, 200MHz) delta: 7.13 (2H, d, J= 8.4 Hz)5 6.61 (2H, d5 J= 8.4 Hz), 3.41 (2H, s), 2.45 (8H, bm), 2.27 (3H, s); m/e = 206 (M+l).To a stirred solution of 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g, 15.57 mmol) in acetic acid: concentrated HCl (32:32 niL) at 10 0C was added NaNO2 (1.30 g,18.78 mmol) in water (16 mL) and stirred for 10 min. Freshly prepared SnCl2^H2O (11.75 g, 51.97 mmol) in concentrated HCl (32 mL) was added at 10 0C. The temperature of the reaction mixture was allowed to rise to room temperature and maintained there for 4hr. After filtering the reaction mixture, the precipitate was washed with water and the solid obtained was dried under reduced pressure to obtain l-(4-hydrazmobenzyl)-4- methylpiperazine (3.4 g). 1HNMR (CD3OD, 200MHz) delta: 7.66 (2H, d, J= 8.4 Hz), 7.13 (2H, d, J= 8.4 Hz), 4.46 (2H, s), 3.72 (8H5 bm), 3.11 (3H5 s);To a solution of l-(4-hydrazinobenzyl)-4-methylpiperazine (3.4 g, 13.25 mmol) in ethanol (50 mL) were added piperidone. HCl (2.51 g, 18.55 mmol). The reaction temperature was raised to 90 0C and continued stirring for 2 hrs. The progress of the reaction was monitored by TLC and upon completion of the reaction the mixture was cooled to rt and HCl gas was bubbled through the reaction mixture at 0 0C. After the reaction mixture was saturated with HCl, the temperature was raised to 90 0C again and continued stirring for 2hrs. The ethanolic HCl was removed under reduced pressure and the pH of the reaction mixture was adjusted to 12.0 with 10% NaOH solution. The mixture was partitioned between 20% MeOH: DCM and water (35 mL) and the organic layer was separated, dried over Na2SO4 filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5- tetrahydro-lNo.-pyrido[4,3-&]indole (1 g). 1HNMR(CD3OD5 200MHz) delta: 7.31 (IH, s), 7.27 (IH, d, J= 8.6 Hz), 7.06 (IH, d, J= 8.6 Hz), 4.01 (2H5 s), 3.60 (2H, s), 3.21 (8H5 bm), 2.86 (4H5 m), 2.28 (3H, s); m/e = 285 (M+l).To a solution of 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5-tetrahydro-li- pyrido[4,3-delta]indole(0.5 g,1.76 mmol) in DMF (15 mL) at rt was added Example 7 (0.567 g, 2.64 mmol) and K2CO3 (0.731 g, 5.28 mmol). The reaction temperature was raised to 100 0C and continued stirring for 12hr. The progress of the reaction was monitored by TLC and upon completion of the reaction DMF was removed under reduced pressure. The reaction mixture was partitioned between ethyl acetate (100 mL) and water (80 mL) and the organic layer was separated, dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave methyl 2-{8-[(4- methylpiperazin-1 -yl)methyl]-l 53s4,5-tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5- carboxylate (0.15 g). 1HNMR (DMSO-D6, 200MHz) delta: 8.84 (2H, s), 7.94 (lH,s), 7.67 (IH, d, J= 8.6 Hz), 7.54 (IH, d, J= 8.6 Hz), 5.01 (2H, s), 3.80-3.01 (1OH, m), 2.87 (3H, s); m/e = 421 (M+l).To a 00C solution of methyl 2-{8-[(4-methylpiperazin~l-yl)methyl]-l,3,4,5- tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5-carboxylate (0.1 g) in MeOH: DCM (5:2 mL) was added 50% aqueous hydroxylamine solution (2 mL) and to the mixture was added a solution of NaOH (0.08 g) in water (1 mL). The reaction mixture was stirred at room temperature for lhr and the progress of the reaction was monitored by TLC and upon completion of the reaction the solvent was removed under reduced pressure. The pH of the mixture was adjusted to 7.5 using IN HCl and the obtained solid was filtered and washed with water followed by diethyl ether. After filtering, t…

109-01-3, 109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; MIKANA THERAPEUTICS, INC.; WO2006/88949; (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.13754-38-6,1-Benzoylpiperazine,as a common compound, the synthetic route is as follows.

Manufacturing Example 9 (4-(2-hydroxy-2-methylpropyl)piperazine-1-yl)phenylmethanone 500 mg (2.63 mmol) 1-benzoylpiperazine and 1.10 g (7.96 mmol, 3.0 eq.) potassium carbonate were suspended to 20 ml acetonitrile at room temperature. After adding 570 mg (7.90 mmol, 3.0 eq.) isobutylene oxide, it was heated at reflux and stirred overnight. After cooling to room temperature and adding 30 ml purified water, it was extracted twice with 30 ml ethylacetate. After collecting organic layer and drying with anhydrous magnesium sulfate, it was concentrated with decompression. The obtained residue was purified by chromatography using silicagel (mobile phase: dichloromethane/methanol=20:1) and 276 mg (40%) target compound as light-yellow solid was yielded. 1H NMR (400 MHz, DMSO-d6) 1.10 (6H, s), 2:23 (2H, s), 2.43-2.52 (2H, m), 2.53-2.62 (2H, m), 3.35-3.45 (2H, m), 3.55-3.65 (2H, m), 4.13 (1H, s), 7.35-7.38 (2H, m), 7.43-7.46 (3H, m)

13754-38-6, 13754-38-6 1-Benzoylpiperazine 762654, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; YANG JI CHEMICAL CO., LTD.; US2012/190689; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

122323-88-0, Methyl piperazine-2-carboxylate dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Reference Example 2 A solution of 3,4,5-trimethoxybenzoyl chloride (10.9 g) in dichloromethane (100 ml) is added dropwise taking one hour, under ice-cooling while stirring, to a mixture of methyl piperazine-2-carboxylate dihydrochloride (10.24 g), triethylamine (18.7 g) and dichloromethane (200 ml). The reaction mixture is poured into ice-water, followed by extraction with dichloromethane. The organic layer is washed with water, dried and the solvent is distilled off under reduced pressure. Crystals obtained from the residue are recrystallized from ethyl acetate and hexane to afford methyl 4-(3,4,5-trimethoxybenzoyl)piperazine-2-carboxylate (9.6 g) as colorless needles, m.p. 113-114C., 122323-88-0

122323-88-0 Methyl piperazine-2-carboxylate dihydrochloride 2760425, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Takeda Chemical Industries, Ltd.; EP368670; (1990); 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.373608-48-1,tert-Butyl 4-(3-aminopropyl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

EXAMPLE 17[4-(Benzo[b]thiophen-2-yl)-5-methyl-pyrimidin-2-yl]-[3-(piperazin-1-yl)-propyl]-amine; 4-(3-Aminopropyl)-piperazine-1-carboxylic acid tert-butyl ester (261 mg, 1.07 mmol) is added to a stirred suspension of 4-(benzo[b]thiophen-2-yl)-2-chloro-5-methyl-pyrimidine (140 mg, 0.537 mmol) and diisopropylethylamine (140 muL, 0.805 mmol) in anhydrous 1,4-dioxane (3.5 mL) at ambient temperature under nitrogen. The resultant mixture is heated in an oil bath at 95 C. for 36 hours. At ambient temperature the mixture is concentrated and chromatographed on silica gel, eluting with 2 M NH3/CH3OH in dichloromethane 0-6%, to give 4-{3-[4-(benzo[b]thiophen-2-yl)-5-methyl-pyrimidin-2-yl]-amino-propyl}-piperazine-1-carboxylic acid tert-butyl ester as a white solid (178 mg, 70% yield).TFA (1 mL) is added to a stirred solution of the above product (168 mg, 0.359 mmol) and triethylsilane (0.172 mL, 1.08 mmol) in anhydrous 1,2-dichloroethane (3 mL) at ambient temperature under nitrogen. The resultant solution is allowed to stir for 8 hours. After concentration, the crude product is suspended in CH3OH (5 mL)/dichloromethane (3 mL) then treated with 2.5 N lithium hydroxide (LiOH) (0.43 mL) before it is chromatographed on silica gel, eluting with 2 M NH3/CH3OH in dichloromethane 5-20%, to give the title compound as a yellowish solid (132 mg, 100% yield). ES+(m/z) 368 [M+H]., 373608-48-1

The synthetic route of 373608-48-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Dahnke, Karl Robert; Lin, Ho-Shen; Richett, Michael Enrico; Shih, Chuan; Wang, Q May; Zhang, Bo; US2008/306082; (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.31166-44-6,1-Cbz-Piperazine,as a common compound, the synthetic route is as follows.

General procedure: To a 0.25 M solution of 28 (1.0 eq.) in DMF, secondary amine (1.2 eq.), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.2 eq.), and HOBt.H2O (1.2 eq.) were added. The mixture was stirred at room temperature for 16 hours, then poured into water (20 x DMF volume), and extracted with EtOAc (x3). The combined organic layer was washed with brine, and dried over anhydrous Na2SO4. After evaporation, the resulting residue was purified by silica gel chromatography (MeOH/CHCl3) to afford the product.

31166-44-6, As the paragraph descriping shows that 31166-44-6 is playing an increasingly important role.

Reference£º
Article; Nakano, Hirofumi; Hasegawa, Tsukasa; Imamura, Riyo; Saito, Nae; Kojima, Hirotatsu; Okabe, Takayoshi; Nagano, Tetsuo; Bioorganic and Medicinal Chemistry Letters; vol. 26; 9; (2016); p. 2370 – 2374;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

883554-88-9, 4-Carbamoyl-piperazine-1-carboxylic acid tert-butyl ester is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

883554-88-9, The compound 4-carbamoyl-piperazine-1-carboxylate (0.16g, 0.7mmol) was dissolved in dichloromethane(2mL) was added HCl The ethyl acetate solution (4M, 2mL), stirred at rt for 30min, the solvent was removed togive 0.16g of white solid: piperazin-1-carboxamide hydrochloride Salt, yield: 100%.

As the paragraph descriping shows that 883554-88-9 is playing an increasingly important role.

Reference£º
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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.57260-71-6,tert-Butyl piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

To a stirred solution of tert-butyl piperazine-l-carboxylate 4 (1 g, 5.38 mmol) in CH2C12 (15 mL) at 0 C, were added 2-bromoacetyl bromide (864 mg, 4.3 mmol) and TEA (1 mL, 7.53 mmol). The reaction mixture was warmed to RT and stirred for 4 h. The mixture was quenched with water (50 mL) and extracted with CH2C12 (2 x 40 mL). The combined organic extracts were washed with brine (20 mL), dried (Na2S04), filtered and concentrated under reduced pressure. The crude was purified (silica gel; eluting 25% EtOAc/ hexanes) to afford compound 2 (900 mg, 54%) as pale yellow solid. 1H MR (500 MHz, DMSO-i): delta 4.16 (s, 2H), 3.47-3.42 (m, 4H), 3.38-3.35 (m, 2H), 3.31-3.29 (m, 2H), 1.41 (s, 9H); LC-MS (ESI): m/z 328.1 (M+ + Na)., 57260-71-6

As the paragraph descriping shows that 57260-71-6 is playing an increasingly important role.

Reference£º
Patent; PHARMAKEA, INC.; ROWBOTTOM, Martin W.; HUTCHINSON, John Howard; CALDERON, Imelda; (202 pag.)WO2016/144703; (2016); 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.74879-18-8,(S)-(+)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

74879-18-8, Intermediate 16 (3S)-3-Methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine [0217][0218](2S)-2-Methylpiperazine (15 g, 150 mmol) was dissolved in tetrahydrofuran (300 mL) and the solution was cooled down to 0 C. Sodium hydroxide (150 mL, 449 mmol) was added, then 4-(trifluoromethyl)benzenesulfonyl chloride (40 g, 164 mmol) (dissolved in 200 ml THF) was added dropwise and the resulting mixture was stirred for 1 h. Further 4-(trifluoromethyl)benzenesulfonyl chloride (0.06 eq, 2.2 g) was added and mixture stirred for 10 min. The mixture was diluted with DCM (500 ml) and water (500 ml) and stirred for 5 min. The phases were separated, the aqueous layer was extracted with DCM (1000 ml) and the organic phases concentrated under reduced pressure. The residue was taken-up with 1 M HCl (500 ml) and washed with DCM in order to extracted impurities. The aqueous phase was basified to pH=9 with NaOH 3M, extracted with DCM (3¡Á500 ml) and the combined organic phases dried over Na2SO4 before the solvent was removed under reduced pressure to give the title compound (30 g).[0219]LCMS (low pH) m/z (ES) 309 [M+H]+[0220]1H NMR (400 MHz, CDCl3) delta 1.06 (d, J=7.2 Hz, 3H), 1.94 (t, J=10.4 Hz, 1H), (td, J=11.2, 4.0 Hz, 1H), 2.88-3.07 (m, 3H), 3.66 (m, 2H), 7.83 (d, J=8.4 Hz, 2H), 7.90 (d, J=8.4 Hz, 2H) ppm

The synthetic route of 74879-18-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; CONVERGENCE PHARMACEUTICALS LIMITED; Heer, Jag Paul; Cridland, Andrew Peter; Norton, David; US2013/72499; (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.25057-77-6,1,2-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

5-Chloro-N-[5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (390 mg, 1.00 mmol) was added in one portion to 1,2-dimethyl-piperazine (228 mg, 2.00 mmol) in anhydrous dimethylsulfoxide (2.00 ml) at 25 C. The resulting solution was stirred at ambient temperature for 2 h. The residue was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH to afford impure material. The concentrated eluent was purified by silica column chromatography, eluting with a gradient of 0 to 10% 7M NH3/MeOH in DCM. Pure fractions were evaporated to dryness to afford the title compound (392 mg, 84%) as a yellow solid. 1H NMR (399.902 MHz, DMSO) delta 1.08 (3H, d), 2.06-2.12 (1H, m), 2.18 (1H, td), 2.23 (3H, s), 2.77-2.88 (2H, m), 3.14-3.21 (1H, m), 3.75 (6H, s), 4.32 (2H, t), 5.08 (2H, s), 5.84 (1H, s), 6.44 (1H, t), 6.59 (2H, d), 8.34 (1H, s), 8.71 (1H, s), 10.79 (1H, s), 11.35 (1H, s). MS: m/z 468 (MH+). Mean of n=1, FGFR Kinase assay-Caliper Echo Dosing, IC50 0.0015 muM.

25057-77-6, As the paragraph descriping shows that 25057-77-6 is playing an increasingly important role.

Reference£º
Patent; ASTRAZENECA AB; US2008/153812; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics