Month: June 2021

132710-90-8, 1-Boc-4-(3-hydroxypropyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of tert-butyl 4-(3 -hydroxypropyl)piperazine- 1 -carboxylate (1.52 g, 6.2 mmol), Ph3P (2.46 g, 9.4 mmol), 12 (2.40 g, 9.4 mmol) and imidazole (1.28 g, 18.6 mmol) in DCM (100mL) was stirred at room temperature for 5 h and then diluted with DCM (200 mL). The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated. The residue was purified by chromatography (PE : EtOAc = 5 : 1) to provide tert-butyl 4-(3- iodopropyl)piperazine- 1 -carboxylate (1 .10 g, 50%) as a colorless oil.

132710-90-8, As the paragraph descriping shows that 132710-90-8 is playing an increasingly important role.

Reference：
Patent; PRINCIPIA BIOPHARMA, INC.; VERNER, Erik; BRAMELD, Kenneth Albert; WO2015/120049; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

39539-66-7, EXAMPLE 1 4-(5-Chloropyridin-2-yl)-3-methyl-5-[(4-methylpiperazin-1-yl)carbonyl]oxy-1,2,4-triazole 50 g (0.24 mol) of 4-(5-chloropyridin-2-yl)-5-hydroxy-3-methyl-1,2,4-triazole are dissolved or suspended in 1 litre of absolute tetrahydrofuran. The sodium hydride, degreased with toluene, is added thereto from 10.8 g of a 55% sodium hydride dispersion and the mixture is stirred for 1 hour at ambient temperature. Then 39 g (0.24 mol) of freshly distilled 1-chlorocarbonyl-4-methyl-piperazine (Bp17: 120-124 C.) are added dropwise thereto and the mixture is stirred for a further 5 hours whilst moisture is excluded. The resulting suspension is concentrated by evaporation in vacuo and the residue is carefully mixed with water and neutralised. The solution containing the carbamate is extracted several times with methylene chloride and the organic phase is washed with water, dried and concentrated. The residue is triturated with ether and 55 g (68% of theory) of the title compound are obtained in the form of crystals, m.p. 121-122 C. 12.5 g of this base are dissolved in 100 ml of methanol and 4.3 g of fumaric acid are added hot. On cooling, the hemifumarate crystallises out, m.p. 173-175 C. (yield: 17 g). The compound is highly water-soluble; pH of the solution 3.5. The starting compound, 4-(5-chloropyridin-2-yl)-5-hydroxy-3-methyl-1,2,4-triazole, is obtained as follows:

39539-66-7 4-Methylpiperazine-1-carbonyl chloride 3016935, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Boehringer Ingelheim KG; US4732900; (1988); 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.216144-45-5,4-(4-Methylpiperazin-1-yl)benzylamine,as a common compound, the synthetic route is as follows.

Stage 3: methyl 4-[2-[4-(4-methylpiperazin-1-yl)benzyl]amino-4-oxoquinazolin-3(4H)-yl]butanoateTriethylamine (0.4 mL) and [4-(4-methylpiperazin-1-yl)benzyl]amine (300 mg) are successively added to a solution of methyl 4-(2-chloro-4-oxoquinazolin-3(4H)-yl)butanoate (140 mg) in tetrahydrofuran (3 mL). The mixture is stirred at ambient temperature for 24 hours then water and ethyl acetate are added. After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40 C. Purification by flash chromatography on silica gel (eluent: dichloromethane/methanol 95:5) produces the expected compound in the form of beige crystals (131 mg, 58% yield from Stage 1).MS/LC: calculated MM=449.2; m/z=450.2 (MH+)NMR (1H, 400 MHz, DMSO-d6): delta 1.85 (t, 2H), 2.21 (s, 3H), 2.40 (m, 6H), 3.08 (m, 4H), 3.54 (s, 3H), 4.05 (t, 2H), 4.54 (d, 2H), 6.86 (AB, 2H), 7.08 (t, 2H), 7.18 (AB, 1H), 7.25 (AB, 2H), 7.48 (t, 1H), 7.52 (t, 1H), 7.89 (AB, 1H).

216144-45-5, The synthetic route of 216144-45-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; SOCIETE DE CONSEILS DE RECHERCHES ET D’APPLICATIONS SCIENTIFIQUES (S.C.R.A.S.); US2010/144714; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13349-91-2, 1-(2,2,2-Trifluoroethyl)piperazine dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

In a 5 mL glass microwave vial equipped with a magnetic stirring bar and nitrogen flow at room temperature was placed methyl 4-bromo-1-(4-bromo-5-(isopropylthio)thiazol-2- yl)-3-methyl-1 H-pyrazole-5-carboxylate prepared as described above with respect to Compound 1 (300 mg, 0.659 mmol), 1-(2,2,2-trifluoroethyl)piperazine hydrochloride (135 mg, 0.659 mmol), XantPhos (38.1 mg, 0.066 mmol) and Cs2C03(1.07 g, 3.30 mmol),nitrogen and vacuum cycles were performed (2x). Nitrogen gas was bubbled through dioxane (3 mL), which was then added to the microwave vial, followed by the addition of the catalyst RuPhos Palladacycle (53.8 mg, 0.066 mmol). The vial was capped and placed in an oil bath at 105 C for 16 h. The solvent was evaporated under vacuum and the crude product was purified by flash chromatography on silica gel (dry packing) using a solution of EtOAc in hexanes (10 to 30% gradient), affording the title compound (123 mg, 0.227 mmol, 34%) as yellow oil., 13349-91-2

The synthetic route of 13349-91-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; BANTAM PHARMACEUTICAL, LLC; SIDDIQUI, Arshad, M.; CIBLAT, Stephane; DERY, Martin; CONSTANTINEUA-FORGET, Lea; GRAND-MAITRE, Chantal; BRUNEAU-LATOUR, Nicolas; SHIPPS, Gerald, W.; COOPER, Alan, B.; OZA, Vibha; KOSTURA, Matthew, W.; LUTHER, Michael; LEVINE, Jedd; (174 pag.)WO2018/102453; (2018); 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.1001180-21-7,(R)-tert-Butyl 4-(5-methyl-7-oxo-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

A flask was equipped with a thermocouple, mechanic stirrer, a nitrogen inlet and drying tube. To the flask was added (R)-tert-buty 4-(5-methyl-7-oxo-6,7-dihydro-5H- cyclopenta[i ]pyrimidin-4-yl)piperazine-l -carboxylate (46.0 g, 139 mmol) followed by dichloromethane (1.10 L) and RuCl(TsDACH) catalyst (1.50 g, 2.80 mmol) with nitrogen degassing (gas dispersion tube) and agitation at room temperature. To the mixture was added triethylamine (23.0 mL, 167 mmol) with degassing. Formic acid (7.40 mL, 195 mmol) was slowly added to the mixture at a rate of about 1 mL/min. Good agitation with stirring was maintained until complete consumption of starting material (about 8-12 hr) as determined by HPLC analysis. The reaction was quenched with saturated sodium bicarbonate (2.00 vol., 100 mL), the layers were separated and the aqueous layer was discarded. The organic layer was washed with saturated sodium bicarbonate, saturated ammonium chloride and brine (2.00 vol., 100 mL each). The organics were dried over sodium sulfate, filtered and solvent exchanged into methanol. The methanolic solution (5.00 vol.) of crude product was charged with 50 wt % SiliaBond Thiol (Silicycle, Inc.) and 20 wt% Charcoal. The mixture was heated to about 50 C and maintained at that temperature with good stirring overnight. The mixture was cooled to room temperature, filtered over a pad of Celite and then polish filtered through a 0.45 micron filter. The mixture was distilled to a minimum working volume and concentrated under reduced pressure to afford the product (44.0 g, 95 % yield), as a 96:4 mixture of trans/cis diastereomers) as solid. Trace amount of Ru metal was measured by ICP-EOS and found that the product contained less than about 20 ppm Ru. The product was purified by preparative HPLC under the following conditionsor crystallization from ethyl acetate/heptane to yield 98.4 % pure product, 97.7 % de with about 100% ee., 1001180-21-7

The synthetic route of 1001180-21-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ARRAY BIOPHARMA INC.; GENENTECH, INC.; LANE, Jonathan W.; REMARCHUK, Travis; SHAKYA, Sagar; SPENCER, Keith L.; STENGEL, Peter J.; WO2013/173736; (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.55276-43-2,1-Methanesulfonylpiperazine,as a common compound, the synthetic route is as follows.,55276-43-2

Example 17 (2R,3R)-2-(2,4-Difluorophenyl)-3-[4-(methanesulphonyl)piperazin-1-yl]-1-(1H-1,2,4-triazol-1-yl)butan-2-ol: The epoxide IV (300 mg, 1.19 mmol) and LiClO4 (235 mg, 1.43 mmol) were dissolved in 12 mL dry acetonitrile and 1-methanesulfonylpiperazine (190 mg, 1.79 mmol) was added. The mixture was heated to reflux for 4 days, cooled and the solvent evaporated. The residue was dissolved in dichloromethane and then washed with water and brine. The solution was dried over Na2 SO4 and the solvent evaporated. The crude reaction products were eluted through a silica gel column using 3% MeOH/97% EtOAc as eluent to give the title compound (180 mg, 36%) as a colorless solid. m.p.: 83-85 C. 1 H NMR (CDCl3) delta: 0.91 (d, J=6.4 Hz, 3H), 2.56-2.61 (m, 2H), 2.80 (s, 3H), 3.02-3.18 (m, 3H), 3.22-3.30 (m, 4H), 4.89 (s, 2H), 4.93 (s, 1H), 6.66-6.79 (m, 2H), 7.35-7.48 (m, 1H), 7.79 (s, 1H), 7.88 (s, 1H). FAB-MS: 415.9 (MH+), C17 H23 F2 N5 O3 S 415.45

The synthetic route of 55276-43-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Synphar Laboratories, Inc.; Taiho Pharmaceuticals Co., Ltd.; US6153616; (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.55121-99-8,(4-Aminophenyl)(4-methylpiperazin-1-yl)methanone,as a common compound, the synthetic route is as follows.

55121-99-8, 2-Methanesulfmyl-7-(2-methoxy-phenyl)-pyrrolo[2, 1 -f] [ 1 ,2,4]triazine (125.0 mg, 0.0004350 mol), N,N-Diisopropylethylamine (0.114 niL, 0.000652 mol) and (4-Amino- phenyl)-(4-methyl-piperazin-l-yl)-methanone (0.191 g, 0.000870 mol) were dissolved in l-Methoxy-2-propanol (1.2 rnL, 0.013 mol) and the reaction was irradiated at 300 watts, 1800C for 40 minutes or until HPLC showed consumption of starting material. The reaction mixture was then reduced en vacuo and the product was isolated and purified by Gilson prep HPLC to afford 73.56 mg of {4-[7-(2-Methoxy-phenyl)-pyrrolo[2,l- f][l,2,4]triazin-2-ylamino]-phenyl}-(4-methyl-piperazin-l-yl)-methanone as a lyophilized powder. (M+H) = 443.8. 1H NMR (400 MHz, DMSO, d6) delta 9.74 (s, IH), 9.00 (s, IH), 7.76 (m, 3H), 7.48 (m, IH), 7.33 (d, 2H, J = 8.64 Hz), 7.23 (d, IH, J = 8.28 Hz), 7.13 (t, IH, J = 7.48 Hz), 6.97 (m, 2H), 3.81 (s, 3H), 3.06 (m, 4H), 3.26 (m, 2H), 3.07 (m, 2H), 2.83 (s, 3H).

55121-99-8 (4-Aminophenyl)(4-methylpiperazin-1-yl)methanone 231408, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; CEPHALON, INC.; BRESLIN, Henry J.; CHATTERJEE, Sankar; DIEBOLD, James L.; DORSEY, Bruce D.; DUNN, Derek; GINGRICH, Diane E.; HOSTETLER, Greg A.; HUDKINS, Robert L.; HUNTER, Rachael; JOSEF, Kurt; LISKO, Joseph; MESAROS, Eugen F.; MILKIEWICZ, Karen L.; OTT, Gregory R.; SUNDAR, Babu G.; THEROFF, Jay P.; THIEU, Tho; TRIPATHY, Rabindranath; UNDERINER, Theodore L.; WEINBERG, Linda; WELLS, Gregory J.; ZIFICSAK, Craig A.; WO2010/71885; (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.182618-86-6,1-Boc-4-(4-Nitrophenyl)piperazine,as a common compound, the synthetic route is as follows.

To a stirred solution of 61 tert-butyl 4-(4-nitrophenyl)piperazine-1-carboxylate (6.50 g, 21.17 mmol, 1.0 eq) in 100 mL of 6 ethanol: 7 water (1:1) mixture were added 67 NH4Cl (11.40 g, 211 mmol, 10 eq) and Fe(0) (4.70 g, 84.68 mmol, 4.0 eq). Reaction mixture was heated at 80 C. for 4 h. Progress of reaction was monitored by LCMS. Upon the consumption of starting material, solvent was removed under reduced pressure. Aqueous layer was basified with saturated solution of 68 sodium carbonate and extracted with ethyl acetate (200 mL×2). Combined organic layer was washed with 50 mL of brine solution, dried over anhydrous Na2SO4 and concentrated under reduced pressure to obtain 4.0 g (68%) of 69 tert-butyl 4-(4-aminophenyl)piperazine-1-carboxylate.LCMS: 278 [M+1]+

182618-86-6, As the paragraph descriping shows that 182618-86-6 is playing an increasingly important role.

Reference：
Patent; giraFpharma LLC; Chakravarty, Sarvajit; PHAM, Son Minh; Kankanala, Jayakanth; AGARWAL, Anil Kumar; PUJALA, Brahmam; SONI, Sanjeev; ARYA, Satish K.; PALVE, Deepak; KUMAR, Varun; (360 pag.)US2019/106436; (2019); A1;,
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

General procedure: Method B: Oxalyl chloride (2 M in CH2Cl2) was added dropwiseto an ice-cooled solution of 2 in dry CH2Cl2 under an argon atmosphere. After 1 h, the ice-bath was removed and the reaction batch was stirred overnight at ambient temperature in an atmosphere of Ar. Subsequently the solvent was evaporated in vacuo and the crude acyl chloride was dissolved in dry DMF and added dropwise to a stirred suspension of amine and K2CO3 in dry DMF at 0 °C. The stirring was continued for 1 h and then at ambient temperature overnight. After 20 h the suspension was filtered, the solvent evaporated, the residue taken up in water and extracted with CH2Cl2. The organic layer was washed with 5percent aqueous NaHCO3 and brine.Then it was dried over anhydrous sodium sulfate, filtered and the solvent was evaporated in vacuo yielding the raw quinoline-4-carboxamides 9?11, which were further purified by column chromatography., 934-98-5

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Hochegger, Patrick; Faist, Johanna; Seebacher, Werner; Saf, Robert; Maeser, Pascal; Kaiser, Marcel; Weis, Robert; Bioorganic and Medicinal Chemistry; vol. 25; 7; (2017); p. 2251 – 2259;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

4318-42-7, 1-Isopropylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Method L; General method for the synthesis of 2, 5-diaminopyridines of type L;. Step 1:; A solution of 2-chloro-5-nitropyridine (0.317 g, 1.06 mL, 0. 002mol), N, N- diisopropylethylamine (1.1 equiv), and amine (1.1 equiv) in acetonitrile (40 mL) was refluxed for 24 h. The reaction mixture was cooled to room temperature and concentrated. The brown residue was used without purification.

4318-42-7, As the paragraph descriping shows that 4318-42-7 is playing an increasingly important role.

Reference：
Patent; AMGEN INC.; WO2005/42518; (2005); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics