Month: April 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.129779-30-2,(3R,5S)-rel-tert-Butyl 3,5-dimethylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

To a solution of tert-butyl cis-3,5-dimethylpiperazine-1-carboxylate (Combi-Blocks Inc., San Diego, Calif., USA, 130 g, 580 mmol, 1.0 equiv) and triethylamine (100 mL, 700 mmol, 1.2 equiv) in tetrahydrofuran (1250 mL, 10 mL/g) was added acryloyl chloride (56 mL, 700 mmol, 1.2 equiv) at 0 C. The reaction mixture was stirred for 1 h at 0 C. The reaction mixture was diluted with ethyl acetate (2.0 L) and washed with water (2*500 mL). The organic layer was washed with 1 N aqueous HCl (500 mL), saturated NaHCO3 (500 mL), and brine (500 mL). The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. The crude material was adsorbed to a plug of silica gel and purified by silica gel column chromatography (30-40% EtOAc/hexane) to provide the title compound as off-white solid (140 g, 91%). MS (ESI, +ve ion) m/z: 269.0 [M+1]; 1H NMR (400 MHz, DMSO-d6) delta 6.78-6.72 (ddd, J=16.7, 10.4, 1.5 Hz, 1H), 6.15-6.11 (dt, J=16.6, 1.9 Hz, 1H), 5.70-5.67 (dt, J=10.6, 1.9 Hz, 1H), 4.35-4.25 (m, 2H), 3.82 (d, J=12.5 Hz, 2H), 3.01-2.95 (m, 2H), 1.43-1.42 (d, J=1.6 Hz, 9H), 1.19-1.14 (m, 6H).

129779-30-2, 129779-30-2 (3R,5S)-rel-tert-Butyl 3,5-dimethylpiperazine-1-carboxylate 10822535, apiperazines compound, is more and more widely used in various fields.

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;,
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Piperazines – an overview | ScienceDirect Topics

169447-70-5, (S)-tert-Butyl 2-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

169447-70-5, Preparation 15 (S)-tert-Butyl 4-(4-chlorophthalazin-1-yl)-2-methylpiperazine-1-carboxylate Heat a mixture of 1,4-dichlorophthalazine (7.80 g, 39.2 mmol), (S)-tert-butyl 2-methylpiperazine-1-carboxylate (4.98 g, 24.9 mmol) and triethylamine (10.3 mL, 73.9 mmol) in DMSO (110 mL) at 80 C. for 18 h. Pour the reaction mixture into water, rinsing with EtOAc. Extract with EtOAc. Wash the organic layer with water (2*) and brine, and dry over Na2SO4, and concentrate under reduced pressure. Purify the resulting residue by flash silica gel chromatography (gradient of 20% to 80% EtOAc in hexanes) to provide the title compound (4.13 g, 46%). ES/MS m/z (35Cl) 363.0 (M+1).

The synthetic route of 169447-70-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; ELI LILLY AND COMPANY; US2011/190304; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5317-33-9, 3-(4-Methylpiperazin-1-yl)propan-1-ol is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2.94 g (19 mmol) of 3-(N-methylpiperazine)propan-1-ol and 2.63 g (24.8 mmol) of sodium carbonate are added to a solution of 5.68 g (12.4 mmol) of 2,2,2-trichloro-N-{3-[3-(3,5-difluorophenyl)-6-oxo-6H-pyridazin-1-ylmethyl]phenyl}acetamide in 25 ml of dimethylformamide, and the mixture is stirred at 100 C. for 20 hours. 50 ml of water are added to the reaction mixture, which is then extracted with dichloromethane. The organic phase is dried over sodium sulfate and evaporated. The residue is chromatographed on a silica-gel column with dichloromethane/methanol as eluent: 3-(4-methylpiperazin-1-yl)propyl{3-[3-(3,5-difluorophenyl)-6-oxo-6H-pyridazin-1-ylmethyl]phenyl}carbamate as colourless crystals.

5317-33-9, 5317-33-9 3-(4-Methylpiperazin-1-yl)propan-1-ol 79208, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; MERCK PATENT GESELLSCHAFT MIT BESCHRAeNKTER HAFTUNG; US2011/136819; (2011); A1;,
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76003-30-0,76003-30-0, 1-Boc-2-methyl-3-oxopiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of the product of Example 1, step a (230 mg, 1.08 mmol) in DCM (5 mL) was added trimethyloxonium tetrafluoroborate (194 mg, 1.25 mmol). The reagent slowly dissolved and after stirring overnight all of the starting material was consumed. To this solution was added 2-picolinyl hydrazide (181 mg, 1.29 mmol). After 24 h the reaction was concentrated in vacuo and dissolved in dioxane (2 mL) and saturated aqueous aHC03 solution (2 mL). The mixture was heated for 3 h at 90 C and the dioxane was removed in vacuo and the aqueous layer extracted with DCM and EtOAc. The combined organic extracts were dried over Na2S04 filtered and concentrated in vacuo. Chromatography on Si02 eluting with IPA/EtOAc afforded the title compound (150 mg, 44%).

As the paragraph descriping shows that 76003-30-0 is playing an increasingly important role.

Reference£º
Patent; JANSSEN PHARMACEUTICA NV; ANDRES GIL, JOSE IGNACIO; LETAVIC, MICHAEL A; RECH, JASON C; RUDOLPH, DALE A; SOYODE-JOHNSON, AKINOLA; CHROVIAN, CHRISTA C; (158 pag.)JP2017/527588; (2017); 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.129799-15-1,Methyl 1-Boc-piperazine-2-carboxylate,as a common compound, the synthetic route is as follows.

Step 1 : 1-tert-Butyl 2-methyl 4-(4-fluorophenyl)piperazine-l,2-dicarboxylate (1113) [00386] To a solution of A29-1 (200.00 mg, 0.819 mmol, 1.00 eq) in DCM (5 mL) were added A29-1A (229. 11 mg, 1.64 mmol, 2.00 eq), Cu(OAc)2 (148.70 mg, 0.819 mmol, 1.00 eq), 4A MS (50 mg) and pyridine (0. 13 mL, 1.64 mmol, 2.00 eq). The reaction mixture was stirred at 25 C for 16 hours under oxygen atmosphere. The reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography over silica gel (petroleum ether: ethyl acetate = 1 :0 to 10: 1) to afford the title compound (250 mg, 90% yield). LCMS (ESI): RT = 0.800 min, mass calcd. for C17H23FN2O4 338.16, m/z found 338.9 [M+H] , NMR (400MHz, COCh-d) delta 7.00 – 6.93 (m, 2H), 6.91 – 6.84 (m, 2H), 4.92 – 4.85 (m, 0.5H), 4.73 – 4.66 (m, 0.5H), 4.09 – 3.88 (m, 2H), 3.78 (s, 3H), 3.40 – 3.18 (m, 2H), 2.94 – 2.83 (m, 1H), 2.79 – 2.66 (m, 1H), 1.49 (d, J=16.8 Hz, 9H).

129799-15-1, As the paragraph descriping shows that 129799-15-1 is playing an increasingly important role.

Reference£º
Patent; VIVACE THERAPEUTICS, INC.; LIN, Tracy Tzu-Ling Tang; KONRADI, Andrei W.; VACCA, Joseph; SHEN, Wang; COBURN, Craig; (231 pag.)WO2017/58716; (2017); A1;,
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Piperazines – an overview | ScienceDirect Topics

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

10.0 g Preparation 3a (37.2 mmol,), 8.7 g 2-(4-methylpiperazin-l-yl)ethanol (60.3 mmol) and 15.8 g PPh3 (60.3 mmol) were dissolved in 100 mL dry toluene and then 27 mL DEAD (60.3 mmol, 40 percent solution in toluene) was added dropwise. The mixture was stirred at 50 ¡ãC under argon atmosphere until no further conversion was observed. The volatiles were evaporated under reduced pressure and 100 mL Et20 was added. The precipitated white crystals were filtered off and washed with Et20. The filtrate was concentrated under reduced pressure and purified via flash chromatography using CHCI3 and MeOH as eluents. The resulting light brown oil was crystallized from hexane to give Preparation 3b as an off-white solid. 1H NMR (500 MHz, DMSO-d6) delta: 7.56 (d, 1H), 6.99 (d, 1H), 4.15 (t, 2H), 2.72 (t, 2H), 2.51 (s, 3H), 2.50 (br s, 4H), 2.29 (br s, 4H), 2.13 (s, 3H), 1.29 (s, 12H)

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; LES LABORATOIRES SERVIER; VERNALIS (R&D) LIMITED; BALINT, Balazs; CSEKEI, Marton; SZABO, Zoltan; SZLAVIK, Zoltan; KOTSCHY, Andras; CHANRION, Maia; GENESTE, Olivier; CHEN, I-Jen; DAVIDSON, James Edward Paul; MURRAY, James Brooke; SIPOS, Szabolcs; ONDI, Levente; PROSZENYAK, Agnes; (164 pag.)WO2016/207217; (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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-07-9

General procedure: 2-Substituted piperazine or 2,6-Disubstitutedpiperazine (5.0 mmol) was dissolved in dry dichloromethane(100 mL) and cooled to 0 C. A solution of the appropriate acylatingagent (5.0 mmol) in dichloromethane (20 mL) was added dropwisein 30 min, and then pyridine (7.5 mmol). The reaction mixture waskept into an ice-water bath with stirring 12 h and left at roomtemperature until TLC showed that all the starting material hadreacted. The reaction mixture was evaporated to dryness to obtainthe corresponding monoacyl derivative. Column chromatographygave the pure compound in high yield.1-tert-Butoxycarbonyl-3-methylpiperazine (16) [21]. Theproduct was obtained as a syrup and purified by column chromatographyusing dichloromethane-methanol (15:1) as eluent(750 mg, 75% yield). MS (CI): m/z 201 (20%) [M+H]+. 1H NMR(500 MHz, DMSO-d6) delta 3.75-3.71 (m, 2H), 2.85-2.82 (m, 1H),2.75-2.69 (m, 1H), 2.60-2.54 (m, 3H), 2.39-2.34 (m, 1H), 1.41 (s,9H), 0.96 (d, J 6.3 Hz, 3H). 13C NMR (125 MHz, DMSO-d6) delta 154.5,79.3, 51.2, 50.5, 45.5, 44.4, 28.6, 19,3. HRMS (m/z): calcd forC10H20N2O2 200.1528 [M]+.; found 200.1525.

The synthetic route of 109-07-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Mazzotta, Sarah; Marrugal-Lorenzo, Jose Antonio; Vega-Holm, Margarita; Serna-Gallego, Ana; Alvarez-Vidal, Jaime; Berastegui-Cabrera, Judith; Perez del Palacio, Jose; Diaz, Caridad; Aiello, Francesca; Pachon, Jeronimo; Iglesias-Guerra, Fernando; Vega-Perez, Jose Manuel; Sanchez-Cespedes, Javier; European Journal of Medicinal Chemistry; vol. 185; (2020);,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

3022-15-9, Piperazine-2-carboxylic acid dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a stirring solution of piperazine-2-carboxylic acid dihydrochloride (SMI) (5 g, 24.6 mmol) in 1,4-dioxane (40 mL) were added 5 N NaOH solution (3.5 g, 88.6 mmol) and Boc-anhydride (12.9 mL, 56.6 mmol) at 0 C and the reaction mixture was stirred at RT for 16 h. After consumption of the starting material (by TLC), volatiles were evaporated under reduced pressure. Obtained crude was dissolved in water (50 mL) and extracted with Et20 (2 x 100 mL). Organic layer was acidified with 1 N HC1 solution and extracted with EtOAc (2 x 100 mL). Combined organic layer was dried over Na2S04 and concentrated under reduced pressure to afford crude compound which was triturated with n-pentane to obtain compound 1 (6 g, 74%) as white solid. 1H-NMR: (400 MHz, DMSO-rfe): delta 12.91 (br s, 1H), 4.42 (d, / = 24.8 Hz, 1H), 4.35-4.27 (dd, / = 20.4, 13.6 Hz, 1H),3.82 (s, 1H), 3.66 (d, / = 13.2 Hz, 1H), 2.99-2.79 (m, 2H), 2.79 (br s, 1H), 1.37 (s, 18H). LCMS (m/z): 329.3 [M+-l]

3022-15-9, 3022-15-9 Piperazine-2-carboxylic acid dihydrochloride 2723757, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; APTINYX INC.; KHAN, M., Amin; (75 pag.)WO2018/26782; (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.57260-71-6,tert-Butyl piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Reference Example 78 4-(4-tert-Butoxycarbonylpiperazin-1-yl)benzaldehyde 1-tert-Butoxycarbonylpiperazine (3.00 g) was added to a DMF solution (40 ml) of 4-fluorobenzaldehyde (2.00 g) and sodium carbonate (3.34 g), followed by stirring overnight at 90C. The reaction solution was cooled to room temperature, water was added to the mixture, extracted with ethyl acetate and then dried over sodium sulfate. The solvent was evaporated, the thus obtained residue was purified by silica gel column chromatography, and the fraction obtained from the elude of n-hexane: ethyl acetate = 10:3 was concentrated under reduced pressure to obtain the title compound (3.21 g) as a white solid. 1H-NMR (400 MHz, CDCl3) delta: 1.49 (9H, s), 3.39 (4H, t, J=4.9 Hz), 3.59 (4H, t, J=4.9 Hz), 6.91 (2H, d, J=8.8 Hz), 7.76 (2H, d, J=8.8 Hz), 9.79 (1H, s). ESI-MS m/z: 291 (M+H)+., 57260-71-6

The synthetic route of 57260-71-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1612204; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

78818-15-2, Benzyl 3-oxopiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

78818-15-2, Preparation No.18: 5-Methoxy-3,6-dihydro-2H-pyrazine-l-carboxylic acid benzyl ester; A solution of benzyl 3-oxopiperazine-l-carboxylate (2.50g, 10.67 mmol) in CH2CI2 (100 mL) was cooled to about 0 C and treated with Na2C03 (23.0 g, 217 mmol) for about 10 min. Neat trimethyloxonium tetrafluoroborate (5.50 g, 37.2 mmol) was added in one portion, then the reaction is allowed to warm to RT for about 6 h. The reaction was poured into water (100 mL), and the layers were separated. The aqueous layer was re-extracted with 50 mL CH2CI2 and the combined organic layers were washed with brine (100 mL). The organic layer was dried over sodium sulfate, filtered and concentrated to yield 5-methoxy-3,6-dihydro-2H- pyrazine-l-carboxylic acid benzyl ester (2.5 lg, 95%) as an oil. LC/MS (Table 1, Method a) Rt = 3.00 min, m/z 249.24 (M+H)+”; .H NMR (400 MHz, DMSO-J6) delta ppm 7.36 (m, 5H), 5.16 (s, 2H), 3.96 (s, 2H), 3.68 (s, 3H), 3.54 (s, 2H), 3.47 (m, 2H)

78818-15-2 Benzyl 3-oxopiperazine-1-carboxylate 736777, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ABBOTT LABORATORIES; CUSACK, Kevin, P.; BREINLINGER, Eric, C.; FIX-STENZEL, Shannon, R.; STOFFEL, Robert, H.; WOLLER, Kevin, R.; WO2011/71570; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics