Tag: M.W:100-200

55112-42-0, 4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,55112-42-0

Example 4: Preparation of Zopiclone in CH2CI2[0067] A slurry of l-chlorocarbonyl-4-methyl piperazine hydrochloride(19.627g) in CH2Cl2 (200ml) was stirred mechanically and cooled to 50C. Then tri- ethyl amine (Et3N) (17.7Ig) was added to the slurry over 25 min. During Et3N addition, there was no temperature rise. After Et3N addition ended, DMAP (1.85g) was added to the slurry, and after 1-2 min of stirring, 7-OH-Py (2Og) was added. The slurry changed its appearance at DMAP addition. The reaction mixture was heated to room temperature and stirred for 6h. After 6h the stirring was continued at reflux for Ih. The reaction mixture was cooled to about 200C and water was added (70 ml). Phases were separated, .with an inter-phase left in organic phase. Organic phase was washed with H2O (2×70 ml). Inter-phase was filtered. Organic phase was dried over MgSO4, filtered and the solvent was evaporated to dryness on rotavapor to give zopiclone crude product (28.94 g, yield 95%; purity 98.69% by HPLC).

55112-42-0 4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride 3016934, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2008/2629; (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.74879-18-8,(S)-(+)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

74879-18-8, In a sealed tube, 7-fluoro-2-(2-methylimidazo[l,2-b]pyridazin-6-yl)-4H-pyrido[l,2- a]pyrimidin-4-one (Intermediate 1; 50 mg, 0.169 mmol), and (S)-2-methylpiperazine (68 mg, 0.677 mmol, 4.0 eq.) were stirred in DMSO (2 mL) at 110C overnight. The solvent was removed under high vacuum. The residue was taken up in CH2CI2and washed with an aqueous saturated solution of NaHC03. The organic layer was separated and dried over Na2S04and concentrated in vacuo. The crude was purified by column chromatography (S1O2,CH2Cl2/MeOH=95/5 to 90/10) to afford the title product (40 mg, 63%) as a light yellow solid. MS m/z 376.2 [M+H+].

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

Reference：
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; MCCARTHY, Kathleen Dorothy; METZGER, Friedrich; RATNI, Hasane; (76 pag.)WO2017/81111; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: To a solution of N-methylpiperazine (0.9819mmol) in dry DMF (4mL), triethylamine (0.27mL, 1.9638mmol) and potassium iodide (16.29mg, 0.0981mmol) were added at rt under N2 atmosphere. To the resultant mixture, compound 2 (0.4g, 0.9819mmol) was added and heated at 125C. After the reaction was complete, as indicated by TLC, DMF was evaporated in vacuo. The obtained residue was diluted with 20mL of water. The compound was extracted with CH2Cl2 (3×5mL). The organic layers were collected, washed with saturated brine solution, dried over anhydrous MgSO4 and concentrated in vacuo. The resultant crude was purified by column chromatography [CH2Cl2/MeOH (1-10%)] to get the title compound.

13889-98-0, The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Suresh, Narva; Nagesh, Hunsur Nagendra; Chandra Sekhar, Kondapalli Venkata Gowri; Kumar, Anil; Shirazi, Amir N.; Parang, Keykavous; Bioorganic and Medicinal Chemistry Letters; vol. 23; 23; (2013); p. 6292 – 6295;,
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.5317-33-9,3-(4-Methylpiperazin-1-yl)propan-1-ol,as a common compound, the synthetic route is as follows.,5317-33-9

A solution of MsCl ( 0.80 g, 7.00 mmol) in DCM (10 mL) was added dropwise to a stirred, ice- cold suspension of 3-(4-methylpiperazin-l-yl)propan-l-ol (1.00 g, 6.32 mmol) in DCM (5 mL). The reaction was stirred at room temperature for 2 h before the solvent was removed under vacuum. The crude product (white solid) was used directly without purification (1.4 g, 94% yield). ‘H NMR (500 MHz, CD3OD SPE) S: 4.38 (t, J= 5.9 Hz, 2H), 3.73 (dd, J= 22.6, 16.8 Hz, 8H), 3.44 – 3.38 (m, 2H), 3.13 (s, 3H), 3.02 (s, 3H), 2.31 – 2.23 (m, 2H).

As the paragraph descriping shows that 5317-33-9 is playing an increasingly important role.

Reference：
Patent; ZHEJIANG VIMGREEN PHARMACEUTICALS, LTD; SUN, Sanxing; ZHAO, Long; HU, Chongbo; CHEN, Zhengshu; YE, Jinqi; (0 pag.)WO2020/2969; (2020); 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, (±) -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 22.7wtpercent, optical purity of 92.3percent e. e. , R KaradaOsamuritsu Retrieving salt to theR-isomer of charge (±) in the 2-methyl piperazine, was 88percent. 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 of100percent, an optical purity of 99.5percent e. e. In and, R KaradaOsamuritsu acquisition crystals for (R) -2-methylpiperazine in charge filtrate was 69percent. 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 100percent, an optical purity of 99.6percent e. e. Inand, R KaradaOsamuritsu acquisition crystals for (R) -2- methylpiperazine in charge filtrate was 68percent. Thermometer, vacuum stirrer, four-necked flask 1L equipped with a Dean-Starkapparatus, 33percent (S) -2- methylpiperazine solution 300.0g ((S) -2- methylpiperazine 100.0 g,Quality: Chemistry purity 99.9percent, optical purity of 80.0percent 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 (…, 109-07-9

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

Reference：
Patent; TORAY FINE CHEMICALS COMPANY LIMITED; MORII, SEIJI; NISHIKAWA, TAKESHI; (12 pag.)JP2016/37495; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

57260-71-6, tert-Butyl piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

57260-71-6, General procedure: 1-Boc-piperazine (150 mg, 0.81 mmoles) was dissolved in anhydrous DMF (2 mL) and, under stirring, DIPEA (303 mL, 1.78 mmoles), PyBOP (461 mg, 0.89 mmoles) and 2-thiophenecarboxylic acid (114 mg, 0.89 mmoles) were added at room temperature. After complete conversion of 1-Boc-piperazine monitored by TLC analysis, the solution was diluted with DCM and washed with NaOH 0.5M, brine, HCl 0.1M and brine. Organic phase was dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified by chromatographic column (eluent DCM/MeOH = 96/4) to obtain 10e (188 mg, 79% yield).

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

Reference：
Article; Giannini, Giuseppe; Battistuzzi, Gianfranco; Vesci, Loredana; Milazzo, Ferdinando M.; De Paolis, Francesca; Barbarino, Marcella; Guglielmi, Mario Berardino; Carollo, Valeria; Gallo, Grazia; Artali, Roberto; Dallavalle, Sabrina; Bioorganic and Medicinal Chemistry Letters; vol. 24; 2; (2014); p. 462 – 466;,
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.

In a sealed tube, 2-(2,8-dimethylimidazo[1,2-b]pyridazin-6-yl)-7-fluoro-pyrido[1,2-a]pyrimidin-4-one (Intermediate 2; 33 mg, 0.107 mmol), and (S)-2-methylpiperazine (43 mg, 0.427 mmol, 4.0 eq.) were stirred in DMSO (2 mL) at 120 C. overnight. The solvent was removed under high vacuum. The residue was taken up in CH2Cl2 and washed with an aqueous saturated solution of NaHCO3. The organic layer was separated and dried over Na2SO4 and concentrated in vacuo. The crude was purified by column chromatography (SiO2, CH2Cl2/MeOH=95/5 to 90/10) to afford the title product (18 mg, 43%) as a light yellow solid. MS m/z 390.3 [M+H+]., 74879-18-8

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

Reference：
Patent; Hoffmann-La Roche Inc.; PTC Therapeutics, Inc.; Ratni, Hasane; Green, Luke; Weetall, Maria L.; Naryshkin, Nikolai A.; (33 pag.)US2019/315773; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59878-57-8, 1-(Cyclopropylcarbonyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(Formula 7-6: methyl 4-((4-(cyclopropanecarbonyl)-N-(pyridin-2-yl)piperazine-1-carboxamido)methyl)benzoate)[1011][1012]Compound ofFormula 7-5(methyl 4-((((4-nitrophenoxy)carbonyl)(pyridin-2-yl)amino)methyl)benzoate; 0.40 g, 0.982 mmol) was dissolved in dimethylformamide (10 mL), and then cyclopropyl(piperazin-1-yl)methanone (0.167 mL, 1.17 mmol) was added, and the mixture was heated and stirred at 60 for 2 days. Then, the dimethylformamide was removed under reduced pressure, water was poured into the reaction mixture, and the organic layer was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride aqueous solution, dehydrated with anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified and concentrated by column chromatography (silica; methanol/dichloromethane=5%) to give the desired compound ofFormula 7-6(0.4 g, 96%) in the form of a white oil.

59878-57-8, 59878-57-8 1-(Cyclopropylcarbonyl)piperazine 2064235, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; CHONG KUN DANG PHARMACEUTICAL CORP.; LEE, Changsik; YANG, Hyun-Mo; CHOI, Hojin; KIM, Dohoon; KIM, Soyoung; HA, Nina; LIM, Hyojin; KO, Eunhee; YOON, Seongae; BAE, Daekwon; WO2014/178606; (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.34770-60-0,4-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

( v) 1 -(4- ( [2-Amino-4-(butylamino )-6-methylpyrimidin-5-yl]methyl } -3-methoxyphenyl)-4- methylpiperazin-2-oneTo a solution of of the product from step (iv) (0.144 g, 0.380 mmol) in 1 ,4-dioxane (2 mL) was added Cul (72.0 mg, 0.379 mmol), N,N’-dimethyldiaminoethane (0.0820 mL, 0.763 mmol), 4-methylpiperazin-2-one (87.0 mg, 0.760 mmol), and Cs2C03 (247 mg, 0.760 mmol). The mixture was heated to 100C and stirred for 1 Oh. After cooling, water was added and the resulting mixture was extracted with EtOAc. The combined organic solutions were washed with brine, and then dried (Na2S04). After removal of the solvent in vacuo, the crude residue was purified by silica gel column chromatography to give the title compound as a pale yellow solid (120 mg, 0.291 mmol, 77 %); 1H NMR: 6.90 (1H , d), 6.86 (1H, s,), 6.72 (1H, d), 4.76 (3H, br s), 3.87 (3H, s), 3.68-3.65 (2H, m), 3.63 (2H, s,), 3.32-3.27 (2H, m), 3.26 (2H, s), 2.78-2.75 (2H, m), 2.39 (3H, s), 2.27 (3H, s), 1.45-1.37 (2H, m), 1.26-1.19 (2H, m), 0.85 (3H, t); LC-MS: m/z = 413 [MH+] (T = 1.48 min).

34770-60-0, 34770-60-0 4-Methylpiperazin-2-one 13704283, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Dainippon Sumitomo Pharma Co., Ltd.; ASTRAZENECA AKTIEBOLAG; TOSAKI, Shinya; HORI, Seiji; WO2012/67268; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: To a solution of N-methylpiperazine (0.9819mmol) in dry DMF (4mL), triethylamine (0.27mL, 1.9638mmol) and potassium iodide (16.29mg, 0.0981mmol) were added at rt under N2 atmosphere. To the resultant mixture, compound 2 (0.4g, 0.9819mmol) was added and heated at 125C. After the reaction was complete, as indicated by TLC, DMF was evaporated in vacuo. The obtained residue was diluted with 20mL of water. The compound was extracted with CH2Cl2 (3×5mL). The organic layers were collected, washed with saturated brine solution, dried over anhydrous MgSO4 and concentrated in vacuo. The resultant crude was purified by column chromatography [CH2Cl2/MeOH (1-10%)] to get the title compound.

13889-98-0, The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Suresh, Narva; Nagesh, Hunsur Nagendra; Chandra Sekhar, Kondapalli Venkata Gowri; Kumar, Anil; Shirazi, Amir N.; Parang, Keykavous; Bioorganic and Medicinal Chemistry Letters; vol. 23; 23; (2013); p. 6292 – 6295;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics