Category: 59702-07-7

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

59702-07-7, EXAMPLE 18 4-Methyl-3-oxo-piperazine-1-carboxylic Acid (4-methoxy-7-piperidin-1-yl-benzothiazol-2-yl)-amide Using 4-methoxy-7-piperidin-1-yl-benzothiazol-2-ylamine and 4-methyl-3-oxo-piperazine, the title compound was prepared as yellow solid in 84percent yield. MS: m/e=404(M+H+).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Flohr, Alexander; Jakob-Roetne, Roland; Norcross, Roger D.; Riemer, Claus; US2003/149036; (2003); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

59702-07-7, [0808] To a solution of (8-((5-cyano-4-((2-methoxyethyl)amino )pyridin-2-yl)carbamoyl)-2-( dimethoxymethyl)-5,6, 7,8-tetrahydro-1 ,8-naphthyridin-3-yl)methyl methanesulfonate(intermediate 170, 368 mg, 0.657 mmol) in DCM(2.7 ml) at room temperature was added NEt3 (0.319 ml,2.301 mmol) followed by 1-methylpiperazin-2-one (120 mg,1.052 mmol). The reaction mixture was stirred at room temperaturefor 2 hand partitioned between DCM and water. Thewater layer was extracted multiple times with DCM, thecombined organic layers were dried using Na2S04 , filteredand evaporated. The crude product was purified by silica gelcolunm chromatography using a gradient ofMeOH (0-3percent) inDCM to yield the title compound as a white solid. (UPLC-MS3) tR 0.87 min; ESI-MS 553.3 [M+Ht. 1H NMR (600 MHz,CDCI3 ) ll13.75 (s, lH), 8.20 (s, lH), 7.64 (br s, lH), 7.58 (s,lH), 5.56 (s, lH), 5.23 (d, lH), 4.06-4.01 (m, 2H), 3.70 (br s,2H), 3.63 (t, 2H), 3.50-3.42 (m, 8H), 3.40 (s, 3H), 3.31 (br s,2H), 3.14 (br s, 2H), 2.96 (br s, 3H), 2.87-2.80 (m, 2H), 2.71(br s, 2H), 2.03-1.96 (m, 2H).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Novartis AG; Buschmann, Nicole; Fairhurst, Robin Alec; Furet, Pascal; Knoepfel, Thomas; Leblanc, Catherine; Liao, Lv; Mah, Robert; Nimsgern, Pierre; Ripoche, Sebastien; Xiong, Jing; Han, Bo; Wang, Can; Zhao, Xianglin; US2015/119385; (2015); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

A mixture of N [5-chloro-7- (3-isopropoxyprop-1-yn-1-yl)-1, 3-benzodioxol-4-yl]-7- (3- chloropropoxy) -6-methoxyquinazolin-4-amine (0.22g, 0. 43mmol), triethylamine (0. 29ml, 2.13mmol), 1-methylpiperazin-2-one (0.24g, 2. 13mmol) in 2-methoxyethanol (3ml) was heated to 80 C for 12 hours and then at 100 C for 7 hours. The solvent was removed under reduced pressure and the residue was partitioned between dichloromethane and water. The organic layer was separated, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by flash chromatography on silica eluting with a mixture of 2-8 percent methanol in dichloromethane to give the product as an light orange solid (0.129g, 51percent). NMR Spectrum: (DMSOd6) 1. 18 (d, 6H), 1.98 (m, 2H), 2.52 (t, 2H under DMSO), 2.72 (t, 2H), 2.88 (s, 3H), 3.04 (s, 2H), 3.34 (t, 2H under H20), 3.83 (m, 1H), 3.97 (s, 3H), 4.22 (t, 2H), 4.42 (s, 2H), 6.17 (s, 2H), 7.15 (s, 1H), 7.21 (s, 1H), 7.83 (s, 1H), 8.34 (s, 1H), 9.52 (s, 1H). Mass Spectrum: M+H+ 596 and M+ll 594

59702-07-7, As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/4732; (2004); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

A mixture of N [5-chloro-7- (3-isopropoxyprop-1-yn-1-yl)-1, 3-benzodioxol-4-yl]-7- (3- chloropropoxy) -6-methoxyquinazolin-4-amine (0.22g, 0. 43mmol), triethylamine (0. 29ml, 2.13mmol), 1-methylpiperazin-2-one (0.24g, 2. 13mmol) in 2-methoxyethanol (3ml) was heated to 80 C for 12 hours and then at 100 C for 7 hours. The solvent was removed under reduced pressure and the residue was partitioned between dichloromethane and water. The organic layer was separated, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by flash chromatography on silica eluting with a mixture of 2-8 percent methanol in dichloromethane to give the product as an light orange solid (0.129g, 51percent). NMR Spectrum: (DMSOd6) 1. 18 (d, 6H), 1.98 (m, 2H), 2.52 (t, 2H under DMSO), 2.72 (t, 2H), 2.88 (s, 3H), 3.04 (s, 2H), 3.34 (t, 2H under H20), 3.83 (m, 1H), 3.97 (s, 3H), 4.22 (t, 2H), 4.42 (s, 2H), 6.17 (s, 2H), 7.15 (s, 1H), 7.21 (s, 1H), 7.83 (s, 1H), 8.34 (s, 1H), 9.52 (s, 1H). Mass Spectrum: M+H+ 596 and M+ll 594

59702-07-7, As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/4732; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, This compound was prepared according to the procedure described for the synthesis of Example 187 using methylpiperazin-2-one in place of L-proline-tert-butyl ester. Into a 50-mL round-bottom flask, was placed a solution of (S)-N1-methyl-N1-(2-oxoethyl)-N3-(4-(piperidin-1-yl)-2-(4-(1,2,3,4-tetrahydronaphthalen-1-ylcarbamoyl)pyridin-2-yl)phenyl)isophthalamide (100 mg, 0.16 mmol, 1.00 equiv) in ethanol (2 mL). This was followed by the addition of a solution of 1-methylpiperazin-2-one (18 mg, 0.16 mmol, 1.00 equiv) in ethanol (2 mL), two drop of acetic acid. To this was added NaBH3CN (20 mg, 0.32 mmol, 2.00 equiv). The resulting solution was stirred for 2 h at room temperature. The resulting solution was diluted with 50 mL of ethyl acetate. The resulting mixture was washed with 2*20 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The crude product (100 mg) was purified by Prep-HPLC with the following conditions (1No.-Waters 2767-3): Column, SunFire Prep C18, 19*150 mm 5 um; mobile phase, water with 0.05percent TFA and CH3CN (22percent CH3CN up to 38percent in 6 min); Detector, Waters2545 UvDector 254&270 nm. 70 mg product was obtained. This resulted in 70 mg (61percent) of (S)-N1-methyl-N1-(2-(4-methyl-3-oxopiperazin-1-yl)ethyl)-N3-(4-(piperidin-1-yl)-2-(4-(1,2,3,4-tetrahydronaphthalen-1-ylcarbamoyl)pyridin-2-yl)phenyl)isophthalamide as a yellow solid. LC-MS (ES, m/z): 728 [M+H]+ H-NMR (300 MHz, DMSO, ppm): 12.25 (s, 1H), 9.18 (d, J=8.4 Hz, 1H), 8.80 (d, J=5.1 Hz, 1H), 8.29 (d, J=13.8 Hz 2H), 7.99 (t, J=6.9 Hz, 2H), 7.86 (d, J=4.8 Hz, 1H), 7.57-7.67 (m, 3H), 7.10-7.28 (m, 5H), 5.25 (d, J=5.4 Hz, 1H), 3.92-3.85 (m, 4H), 3.30-3.54 (m, 10H), 2.78-2.95 (m, 9H), 1.99 (d, J=3.6 Hz, 2H), 1.72-1.80 (m, 6H), 1.60 (s, 2H).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Ardelyx, Inc.; Lewis, Jason G.; Jacobs, Jeffrey W.; Reich, Nicholas; Leadbetter, Michael R.; Bell, Noah; Chang, Han-Ting; Chen, Tao; Navre, Marc; Charmot, Dominique; Carreras, Christopher; Labonte, Eric; (323 pag.)US9301951; (2016); B2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, This compound was prepared according to the procedure described for the synthesis of Example 187 using methylpiperazin-2-one in place of L-proline-tert-butyl ester. Into a 50-mL round-bottom flask, was placed a solution of (S)-N1-methyl-N1-(2-oxoethyl)-N3-(4-(piperidin-1-yl)-2-(4-(1,2,3,4-tetrahydronaphthalen-1-ylcarbamoyl)pyridin-2-yl)phenyl)isophthalamide (100 mg, 0.16 mmol, 1.00 equiv) in ethanol (2 mL). This was followed by the addition of a solution of 1-methylpiperazin-2-one (18 mg, 0.16 mmol, 1.00 equiv) in ethanol (2 mL), two drop of acetic acid. To this was added NaBH3CN (20 mg, 0.32 mmol, 2.00 equiv). The resulting solution was stirred for 2 h at room temperature. The resulting solution was diluted with 50 mL of ethyl acetate. The resulting mixture was washed with 2*20 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The crude product (100 mg) was purified by Prep-HPLC with the following conditions (1No.-Waters 2767-3): Column, SunFire Prep C18, 19*150 mm 5 um; mobile phase, water with 0.05percent TFA and CH3CN (22percent CH3CN up to 38percent in 6 min); Detector, Waters2545 UvDector 254&270 nm. 70 mg product was obtained. This resulted in 70 mg (61percent) of (S)-N1-methyl-N1-(2-(4-methyl-3-oxopiperazin-1-yl)ethyl)-N3-(4-(piperidin-1-yl)-2-(4-(1,2,3,4-tetrahydronaphthalen-1-ylcarbamoyl)pyridin-2-yl)phenyl)isophthalamide as a yellow solid. LC-MS (ES, m/z): 728 [M+H]+ H-NMR (300 MHz, DMSO, ppm): 12.25 (s, 1H), 9.18 (d, J=8.4 Hz, 1H), 8.80 (d, J=5.1 Hz, 1H), 8.29 (d, J=13.8 Hz 2H), 7.99 (t, J=6.9 Hz, 2H), 7.86 (d, J=4.8 Hz, 1H), 7.57-7.67 (m, 3H), 7.10-7.28 (m, 5H), 5.25 (d, J=5.4 Hz, 1H), 3.92-3.85 (m, 4H), 3.30-3.54 (m, 10H), 2.78-2.95 (m, 9H), 1.99 (d, J=3.6 Hz, 2H), 1.72-1.80 (m, 6H), 1.60 (s, 2H).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Ardelyx, Inc.; Lewis, Jason G.; Jacobs, Jeffrey W.; Reich, Nicholas; Leadbetter, Michael R.; Bell, Noah; Chang, Han-Ting; Chen, Tao; Navre, Marc; Charmot, Dominique; Carreras, Christopher; Labonte, Eric; (323 pag.)US9301951; (2016); B2;,
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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

Step 3: A mixture of 50 mg (0.10 mmol) intermediate VI.4 step 2, 14 mg (0.12 mmol) 1 – Methylpiperazin-2-one, 18 mg (0.13 mmol) K2CO3, 3 mg (0.02 mmol) Nal and acetonitrile is heated to 80°C in a sealed tube for 7 h. Additional 14 mg (0.12 mmol) 1 – Methylpiperazin-2-one and 18 mg (0.13 mmol) K2CO3 are added and the mixture is heated to 100°C in a sealed tube for 13 h. After cooling to RT the solvent is evaporated and DCM and water are added. The organic phase is separated, dried, filtered and evaporated yielding 4-[2-[7-bromo-4-[4-fluoro-2-[(1 R)-2,2,2-trifluoro-1 -methyl- ethoxy]anilino]-5-methyl-quinazolin-6-yl]oxyethyl]-1 -methyl-piperazin-2-one. (0642) Yield: 50 mg (Yield 87percent), ESI-MS: m/z = 600 Mu+EtaGamma, R,(HPLC): 1 .06 min (HPLC-M), 59702-07-7

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BLUM, Andreas; WO2015/169677; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, Example 70: (+/-)-4-(c/’s-4-(4-amino-5-(2-phenylchroman-7-yl)-7H-pyrrolo[2,3-d]pyrimidin-7- yl )cyclohexyl)- 1 – methyl piperazin-2-oneTo a mixture of 4-(4-amino-5-(2-phenylchroman-7-yl)-7H-pyrrolo[2,3-d]pyrimidin-7- yl)cyclohexanone (Intermediate AL, 100 mg, 0.23 mmol), 1-methylpiperazin-2-one (137 mg, 0.92 mmol), diisopropyiethylamine (1.84 mmol, 327 uL) in dichloroethane (3 mL), was added sodium triacetoxyborohydride (195 mg, 0.92 mmol). The mixture was stirred at room temperature for 2 h and then concentrated. The resulting residue was purified to a mixture of the cis and trans isomers via reverse phase preparative HPLC (Method S). Preparative silica TLC, eluting with 10percent MeOH in DCM with 0.1 N ammonia, was used to isolate the cis (lower band) isomer. MS m/z 537.3 (M+H+) (Method M).

As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; NOVARTIS AG; IRM LLC, a Delaware Limited Liability Company; CHEN, Bei; FAIRHURST, Robin, Alec; FLOERSHEIMER, Andreas; FURET, Pascal; JIANG, Songchun; LU, Wenshuo; MARSILJE, Thomas, H.; VAUPEL, Andrea; WO2011/64211; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, Example 70: (+/-)-4-(c/’s-4-(4-amino-5-(2-phenylchroman-7-yl)-7H-pyrrolo[2,3-d]pyrimidin-7- yl )cyclohexyl)- 1 – methyl piperazin-2-oneTo a mixture of 4-(4-amino-5-(2-phenylchroman-7-yl)-7H-pyrrolo[2,3-d]pyrimidin-7- yl)cyclohexanone (Intermediate AL, 100 mg, 0.23 mmol), 1-methylpiperazin-2-one (137 mg, 0.92 mmol), diisopropyiethylamine (1.84 mmol, 327 uL) in dichloroethane (3 mL), was added sodium triacetoxyborohydride (195 mg, 0.92 mmol). The mixture was stirred at room temperature for 2 h and then concentrated. The resulting residue was purified to a mixture of the cis and trans isomers via reverse phase preparative HPLC (Method S). Preparative silica TLC, eluting with 10percent MeOH in DCM with 0.1 N ammonia, was used to isolate the cis (lower band) isomer. MS m/z 537.3 (M+H+) (Method M).

As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; NOVARTIS AG; IRM LLC, a Delaware Limited Liability Company; CHEN, Bei; FAIRHURST, Robin, Alec; FLOERSHEIMER, Andreas; FURET, Pascal; JIANG, Songchun; LU, Wenshuo; MARSILJE, Thomas, H.; VAUPEL, Andrea; WO2011/64211; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 95: l-Methyl-4-[4-(methylsuIfonylmethyl)-6-morpholin-4-yl-pyrimidin-2-yl]piperazin-2- oneA mixture of 2-chloro-4-(methylsulfonylmethyl)-6-morpholin-4-yl-pyrimidine (200 mg), l-methylpiperazin-2-one (157 mg) and sodium carbonate (146 mg) in DMA (4 mL) was heated in a microwave reactor at 16O0C for 10 minutes. The reaction mixture was loaded onto a SCX-2 column and product removed with 7N ammonia in methanol. The solution was evaporated to dryness and chromatographed on silica, eluting with 0 – 2.5percent methanol in DCM, to give the desired material (179 mg) as a white solid. Mass Spectrum; MH+ 370NMR Spectrum: 1H NMR (DMSOd6) 52.89 (3H, s), 3.13 (3H, s), 3.38 (2H, t), 3.55 – 3.56 (4H, m), 3.67 – 3.68 (4H, m), 3.93 (2H, t), 4.19 (2H, s), 4.28 (2H, s), 6.28 (IH, s)

59702-07-7, As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2007/80382; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics