Month: September 2020

5625-67-2, Piperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5625-67-2, Boc2O (2.0 mmol, 436mg, 1.0 eq) was added in portions under stirring and cooling on an ice bath to a suspension of piperazin-2-one (2.0 mmol, 200 mg, 1.0 eq) in anhydrous dichloromethane (10.0 mL). The reaction mixture was stirred overnight at room temperature, during which a homogeneous solutionformed. The solvent was evaporated and the solid residue was vacuum-dried tofurnish a yellow solid (300.0 mg, 100%). 1H NMR (300 MHz, CDCl3) delta (ppm): 1.51(s, 9 H); 3.37-3.46 (m, 2 H); 3.66 (t, J= 5.2 Hz, 2 H); 4.12 (s, 2 H); 6.39 (bs, 1 H). 13C NMR (75 MHz, CDCl3) delta (ppm):27.4 (CH2); 28.3 (3 x CH3); 41.2 (CH2); 77.1(CH2); 80.9 (C); 153.9 (C); 168.0 (C). MS (DCI/NH3) m/z: 201.1 [M+H+]; 218.1 [M + NH4+].

The synthetic route of 5625-67-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Chollet, Aurelien; Mori, Giorgia; Menendez, Christophe; Rodriguez, Frederic; Fabing, Isabelle; Pasca, Maria Rosalia; Madacki, Jan; Kordulakova, Jana; Constant, Patricia; Quemard, Annaik; Bernardes-Genisson, Vania; Lherbet, Christian; Baltas, Michel; European Journal of Medicinal Chemistry; vol. 101; (2015); p. 218 – 235;,
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129799-08-2, 1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of l-tert-butyl 3-methyl piperazine- 1, 3 -dicarboxy late (compound I-3a, 1.22 g, 5 mmol) in anhydrous CH2CI2 (15 mL) was added trimethylsilyl isocyanate (634 mg, 5.5 mmol). The resulting mixture was stirred at room temperature for 64 h. The reaction mixture was directly concentrated under reduced pressure to afford crude O l-tert-butyl 03 -methyl 4- carbamoylpiperazine-l,3-dicarboxylate (1.51 g) as a light-yellow foam which was directly used for next step without purification. MS obsd. (ESI+) [(M+H)+]: 288., 129799-08-2

129799-08-2 1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate 2756819, apiperazines compound, is more and more widely used in various.

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; HAN, Xingchun; JIANG, Min; WANG, Yongguang; YANG, Song; (83 pag.)WO2019/129681; (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.76003-29-7,1-Boc-3-Oxopiperazine,as a common compound, the synthetic route is as follows.

76003-29-7, In a 500 mL three-necked flask, 12.70 g (63.0 mmol, 1.0 eq.) of Compound 1 was dissolved in 280 mL of dimethylformamide and cooled to 0 C in an ice bath;1.73 g (73.0 mmol, 1.15 equivalents) of sodium hydride were added and stirred under ice cooling for 1 hour.Then 6.60 mL (69.0 mmol, 1.10 equivalents) of methyl bromoacetate was added via syringe.After further stirring for 20 minutes under ice cooling, the reaction solution was warmed to room temperature. After 18 hours, 10 mL of methanol, 10 mL of deionized water and 180 mL of a saturated sodium chloride solution were added to the reaction solution.The aqueous phase the organic phase was extracted once with 250mL to 140mL extracted three times with ether, and the combined dried over magnesium sulfate, and the solvent was evaporated under reduced pressure.Subsequently, it was removed under reduced pressure at a water temperature of 55 C in 2 hours.Residual dimethylformamide. Obtaining 13.4 g of an orange liquid, purified by flash chromatography using petroleum ether/ethyl acetate 4:1? petroleum ether/ethyl acetate 2:1 as eluent.Got a white solid,Yield: 14.16g (82%, 52.0mmol),White solid,

76003-29-7 1-Boc-3-Oxopiperazine 3157178, apiperazines compound, is more and more widely used in various.

Reference£º
Patent; Shaoxing University; Hu Chunqi; Li Xin; Shi Yaru; Du Wenting; Tong Jie; Su Wanting; Xia Weiqi; (21 pag.)CN108610333; (2018); A;,
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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.

To a solution of(2S,5R)-1-Boc-2,5-dimethylpiperazine (3.5 g, 16.3 mmol, Astatech) in dichloromethane (35 ml), anhydrous triethylamine (4.59 ml, 32.7 mmol) was added and the mixture was cooled to 0 C. in ice-water bath. Acryloyl chloride (1.46 ml, 18.0 mmol) was added dropwise over ?5 min at which point the reaction mixture became yellow and viscous and formation of a white precipitate was observed. Water (10 ml) was added and the mixture was removed from the ice bath and was allowed to stir for 10 min. The organic layer was separated, quickly washed with 2N HCl (40 ml), water and brine, filtered through pad of MgSO4 and concentrated to afford crude tert-butyl (2S,5R)-4-acryloyl-2,5-dimethylpiperazine-1-carboxylate (4.4 g) as yellow oil. This material was redissolved in DCM (40 ml) and TFA (12.6 ml, 163 mmol) was added and the mixture was stirred at rt for 4 h at which point complete deprotection was observed. The mixture was concentrated under reduced pressure and dried under vacuum to afford 1-((2R,5S)-2,5-dimethylpiperazin-1-yl)prop-2-en-1-one 2,2,2-trifluoroacetate (Intermediate 160, ?9 g) as an oil.

548762-66-9 (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate 11745988, apiperazines compound, is more and more widely used in various.

Reference£º
Patent; Amgen Inc.; ALLEN, John Gordon; LANMAN, Brian Alan; CHEN, Jian; REED, Anthony B.; CEE, Victor J.; LIU, Longbin; LOPEZ, Patricia; WURZ, Ryan Paul; NGUYEN, Thomas T.; Booker, Shon; ALLEN, Jennifer Rebecca; CHU-MOYER, Margaret; AMEGADZIE, Albert; CHEN, Ning; GOODMAN, Clifford; LOW, Jonathan D.; MA, Vu Van; MINATTI, Ana Elena; NISHIMURA, Nobuko; PICKRELL, Alexander J.; WANG, Hui-Ling; SHIN, Youngsook; SIEGMUND, Aaron C.; YANG, Kevin C.; TAMAYO, Nuria A.; WALTON, Mary; XUE, Qiufen; US2019/374542; (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 10 Procedure for preparation of (R)-l-amino-N-( l-cyano-2-(4′-((4-cyclopropyl- piperazin-l-yl) methyl) biphenyl-4-yl) ethyl)cyclohexanecarboxamide (PZ1050)The preparation of PZ1050-1: To a solution of 1-cyclopropylpiperazine (2.0 g, 15.9 mmol) in EtOH (20 ml) was added 4-bromobenzaldehyde (2.9 g, 15.9 mmol) and CH3COOH (1.1 g, 19.1mmol). Then this mixture was stirred at room temperature overnight. This mixture was adjusted pH = 9 with NaHC03 and extracted with DCM. Then the organic phase was washed with IN HCI. The organic phase were combined, dried and concentrated in vacuo. The residue was purified by Pre-HPLC to give PZ1050-1 (1.1 g, 23.5%) as yellow solid., 20327-23-5

The synthetic route of 20327-23-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; PROZYMEX A/S; PEDERSEN, John; LAURITZEN, Conni; WO2012/119941; (2012); 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.1235865-77-6,2-((1H-Pyrrolo[2,3-b]pyridin-5-yl)oxy)-4-(4-((4′-chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2-yl)methyl)piperazin-1-yl)benzoic acid,as a common compound, the synthetic route is as follows.

1235865-77-6, (0848) Compound 277J (0.063 g), Compound 277O (0.042 g), 1-ethyl-3-[3-(dimethylamino)propyl]-carbodiimide hydrochloride (0.032 g), and 4-dimethylaminopyridine (0.027 g) were combined in a 4-ml vial with dichloromethane (1.0 ml) and stirred overnight at ambient temperature. The reaction mixture was chromatographed directly without aqueous workup on silica gel with 0-4% methanol in dichloromethane as the eluent. Fractions containing the desired product were concentrated, slurried in acetonitrile, concentrated and dried overnight in a vacuum oven at 80 C. to give the title compound. 1H NMR (500 MHz, pyridine-d5) delta 13.05 (s, 1H), 9.13 (d, 1H), 8.72 (d, 1H), 8.41 (d, 1H), 8.10 (d, 1H), 7.67 (m, 1H), 7.66 (d, 1H), 7.44 (m, 2H), 7.07 (m, 2H), 6.76 (dd, 1H), 6.51 (m, 2H), 4.63 (m, 4H), 4.53 (d, 2H), 3.39 (m, 1H), 3.07 (m, 4H), 2.77 (s, 2H), 2.51 (m, 2H), 2.25 (m, 2H), 2.18 (m, 2H), 2.13 (m, 4H), 2.06 (t, 2H), 1.97 (s, 2H), 1.89 (m, 2H), 1.39 (t, 2H), 0.93 (s, 6H).

The synthetic route of 1235865-77-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; AbbVie Inc.; Catron, Nathaniel; Lindley, David; Miller, Jonathan M.; Schmitt, Eric A.; Tong, Ping; US10213433; (2019); B2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

31166-44-6, 1-Cbz-Piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step A: Benzyl 4-(2-methoxy-2-oxoethyl)piperazine-l-carboxylate.To a solution of benzyl piperazine-1 -carboxylate (0.5 g, 2.270 mmol) and TEA (0.949 mL, 6.81 mmol) in THF (10 mL) was added methyl 2-bromoacetate (0.230 mL, 2.497 mmol) dropwise. The reaction was stirred at 65¡ãC. After 1 hour, the reaction mixture was concentrated, and the residue was partitioned between EtOAc and saturated aqueous NaHC03. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated to generate benzyl 4-(2-methoxy-2-oxoethyl)piperazine-l -carboxylate as a clear oil (0.61 g, 92 percent yield).

31166-44-6, 31166-44-6 1-Cbz-Piperazine 643495, apiperazines compound, is more and more widely used in various.

Reference£º
Patent; AMGEN INC.; BODE, Christiane, M.; CHENG, Alan, C.; CHOQUETTE, Deborah; LEWIS, Richard, T.; POTASHMAN, Michele, H.; ROMERO, Karina; STELLWAGEN, John, C.; WHITTINGTON, Douglas, A.; WO2012/18668; (2012); A1;,
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Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1383146-20-0,(R)-4-(2,4-Dimethoxybenzyl)-3-methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

Synthesis of (R)-l-(2,4-dimethoxybenzyl)-5-ethoxy-6-methyl-l,2,3, 6- tetrahydropyrazine D. Oven dried (115C) sodium carbonate (2.48 g, 23.40 mmol, 2.25 eq.) was placed in a round-bottom flask. The round-bottom flask was backfilled with Ar and then capped with a rubber septum. A solution of (R)-4-(2,4-dimethoxybenzyl)-3-methylpiperazin-2- one C (2.75 g, 10.40 mmol, 1 eq.) in anhydrous DCM (35 mL) was added, followed by freshly prepared triethyloxoniumtetrafluoroborate (2.48 g, 13.05 mmol, 1.25 eq.) in one portion. Thereafter the reaction mixture was stirred further at RT for 45 min to 1 hour, whereupon the reaction mixture was diluted with saturated aqueous NaHC03 (100 mL). The aqueous layer was extracted with DCM (3 x 200 mL). The organic layers were combined, dried over MgS04, filtered and concentrated under reduced pressure to afford 3.1 g of yellow oil. The crude compound was then purified on silica gel (EtOAc/MeOH: 99/1) to afford the desired product D as a pale yellow oil. Yield: 1.44 g, 48 %. LCMS: P = 95 , retention time = 1.8 min, (M+H20+H)+: 311 ; chiral HPLC retention time = 12.3 min, ee > 97 %. 1H-NMR (CDC13): delta 7.23 (d, J= 8.8, 1H), 6.48 (d, J= 8.8, 1H), 6.44 (s, 1H), 4.02 (m, 2H), 3.92 (s, 6H), 3.86 (d, JAB= 14.0, 1H), 3.46 (d, JAB= 14.0, 1H), 3.44 (m, 2H), 3.10 (m, 1H), 2.79 (m, 1H), 2.32 (m, 1H), 1.35 (d, J= 6.8, 3H), 1.24 (t, J= 6.0, 3H)., 1383146-20-0

As the paragraph descriping shows that 1383146-20-0 is playing an increasingly important role.

Reference£º
Patent; EUROSCREEN SA; HOVEYDA, Hamid; DUTHEUIL, Guillaume; FRASER, Graeme; WO2014/154897; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Thermometer, vacuum stirrer, four-necked flask 2L equipped with acooling tube, L- tartaric acid 270g (1.8 mol), acetic acid 108 g (1.8 mol), water 270g was added,was completely dissolved. Then, (¡À) -2- methylpiperazine 300g (3.0 mol), water 300g wasadded, and the reaction was heated 85 C or more, were completely dissolved. Then cooled to6874 C, (R) -2- methylpiperazine and L- diastereomers tartaric was added to precipitatecrystals, allowed to 1 hour aged at that temperature. Then, over a period of 5 hours and cooled to1218 C, and the precipitated crystals were filtered, diastereomeric salt 440g of wet biomass,liquid content 22.7wt%, optical purity of 92.3% e. e. , R KaradaOsamuritsu Retrieving salt to theR-isomer of charge (¡À) in the 2-methyl piperazine, was 88%. Then, charged 644g of water four-necked flask 2L, the resulting crystals 440g ((R) -2-methylpiperazine pure content = 132 g) were added. Furthermore, the addition of calciumhydroxide 162g (2.2mol), then heated to 80 C, and aged at that temperature for 5 hours.Cooled over a period of 2 hours up to 25 C, was filtered off precipitated crystals to remove thewet material crystal of 586g (mainly L- tartaric acid calcium). Get the filtrate 660 g, liberated with L- tartaric acid in the filtrate (R) -2- methylpiperazine were present 130 g. Thermometer, vacuum stirrer, four-necked flask 1L with a cooling tube equippedfiltrate 330g obtained in Reference Example 1 (in the filtrate of (R)-2-methyl-piperazine 65 g)was concentrated under reduced pressure, (R ) concentration of 2-methyl piperazine was distilledoff the water until the 30 percent. Then, toluene 356g was added to the concentrate, a mixedsolution was heated under normal pressure and azeotroped with water and toluene in arms 84 to87 C, excluding the water. Then, toluene was distilled off 212g under reduced pressure. Theconcentrate was cooled to 47 C, (R) -2- methylpiperazine 0.01g was added as a seed crystal toprecipitate crystals, followed by aging for 1 hour at 47 C. Was cooled over 5 hours 05 C,and aged for 2 hours at 06 C. The precipitated crystals were taken out by filtration underreduced pressure, vacuum drying, the crystalline body (R) -2- methylpiperazine was 45gacquired. The resulting quality of (R) -2- methylpiperazine of the crystal body, chemical purity of100%, an optical purity of 99.5% e. e. In and, R KaradaOsamuritsu acquisition crystals for (R) -2-methylpiperazine in charge filtrate was 69%. 1, illustrating the steps from Reference Example 1 to Example 1. Was the first crystallizationfrom ( “1 crystallization” was described as) (described as “crystallization”) last crystallization upto six steps. Compared to the Comparative Example 2 step, short process, was able to get a goodoptically active 2-methylpiperazine of easy nature of handling. Thermometer, vacuum stirrer, four-necked flask 1L with a cooling tube equippedfiltrate 330g obtained in Reference Example 1 (in the filtrate of (R)-2-methyl-piperazine 65 g)was concentrated under reduced pressure, (R ) concentration of 2-methyl piperazine was distilledoff the water until the 30 percent. Then, cyclopentyl methyl ether 356g added to theconcentrated solution, mixed solution was heated to normal pressure and azeotroped water andcyclopentyl methyl ether at 8487 C, except for the water. It was then distilled off cyclopentylmethyl ether 205g under reduced pressure. The concentrate was cooled to 47 C, (R) -2-methylpiperazine 0.01g was added as a seed crystal to precipitate crystals, followed by aging for1 hour at 47 C. Was cooled over 5 hours 05 C, and aged for 2 hours at 06 C. Theprecipitated crystals were taken out by filtration under reduced pressure, vacuum drying, thecrystalline body (R) -2- methylpiperazine was 44g acquired. The resulting quality of (R) -2-methylpiperazine of the crystal body, chemical purity of 100%, an optical purity of 99.6% e. e. Inand, R KaradaOsamuritsu acquisition crystals for (R) -2- methylpiperazine in charge filtrate was 68%. Thermometer, vacuum stirrer, four-necked flask 1L equipped with a Dean-Starkapparatus, 33% (S) -2- methylpiperazine solution 300.0g ((S) -2- methylpiperazine 100.0 g,Quality: Chemistry purity 99.9%, optical purity of 80.0% e.e. ) Were charged. Then stirred withtoluene 586.0g (5.86wt times / (S) -2- methylpiperazine). The solution was heated under normalpressure, arms 84 to 87 was azeotroped with water and toluene in C, except for water only.Then, toluene was distilled off 286g under reduced pressure. The concentrate was cooled to4350 C, (S) -2-methylpiperazine 0.01g was added as a seed crystal to precipitate crystals,followed by aging for 1 hour at 4350 C. Then it cooled over 2 hours to 0 to 5 C, and agedfor 2 hours at 05 C. The precipitated crystals were taken out by filtration under reducedpressure, vacuum drying, the crystalline body (S)-2-methylpiperazine 66.8g was obtained (67%yield). The resulting quality of the crystal of (S) -2- methyl piperazine, the chemical p…

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

Reference£º
Patent; TORAY FINE CHEMICALS COMPANY LIMITED; MORII, SEIJI; NISHIKAWA, TAKESHI; (12 pag.)JP2016/37495; (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.25057-77-6,1,2-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

1,2-Dimethyl-piperazine (0.914 g, 8.00 mmol) and ethyl 4-fluorobenzoate (0.587 mL, 4 mmol) were dissolved in DMA (6 mL) and sealed into a microwave tube. The reaction was heated to 150 C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction mixture was evaporated and the crude product was purified by silica column chromatography, eluting with 5% MeOH in DCM (containing 0.1% 0.880 ammonia). Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.380 g, 36.2%) as a colourless waxy solid. 1H NMR (399.9 MHz, CDCl3) delta 1.15 (3H, d), 1.37 (3H, t), 2.20-2.25 (1H, m), 2.34 (3H, s), 2.37-2.41 (1H, m), 2.61-2.67 (1H, m), 2.87-2.92 (1H, m), 2.99-3.06 (1H, m), 3.58-3.62 (1H, m), 3.65-3.70 (1H, m), 4.33 (2H, q), 6.83-6.87 (2H, m), 7.90-7.94 (2H, m). MS: m/z=263 (MH+).; Ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate used as starting material was prepared as follows:1,2-Dimethylpiperazine (2.284 g, 20.00 mmol) and ethyl 4-fluorobenzoate (1.467 mL, 10 mmol) were dissolved in DMA (12 mL) and sealed in a microwave tube. The reaction was heated to 150 C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction mixture was heated for a further 30 mins at 150 C. and cooled to room temperature. The reaction mixture was evaporated and the crude product was purified by silica column chromatography, eluting with 5% MeOH in DCM with 0.1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.853 g, 32.5%) as a colourless waxy solid. 1H NMR (399.9 MHz, CDCl3) delta 1.14 (3H, d), 1.37 (3H, t), 2.20-2.25 (1H, m), 2.33 (3H, s), 2.34-2.41 (1H, m), 2.62 (1H, t), 2.87-2.91 (1H, m), 2.99-3.05 (1H, m), 3.57-3.62 (1H, m), 3.65-3.70 (1H, m), 4.33 (2H, q), 6.83-6.87 (2H, m), 7.90-7.94 (2H, m). MS: m/z 263., 25057-77-6

25057-77-6 1,2-Dimethylpiperazine 198037, apiperazines compound, is more and more widely used in various.

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