Sep 2021 News Brief introduction of 4-Methyl-1-piperazineacetic acid

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 11; Synthesis of Active Esters Of N-Methyl Piperazine Acetic Acid Via Oxalyl Chloride (Scheme B, FIG. 4B); To a suspension of N-methyl piperazine acetic acid (N-MPAA) (79 mg, 0.5 mmol) in DCM (25 mL) was added a solution of oxalyl chloride (4 mL, 0.8 mmol, 2.0 M solution in DCM) over 10 minute at room temperature. After another 30 minutes of reaction, solvent and excess reagent were removed under reduced pressure to give a white solid (23). A solution of NHS (57 mg, 0.5 mmol) in DCM (25 mL) was added to the solid followed by ss-TBD (390 mg, 1 mmol, 2.6 mmol/g). The resulting solution was sonicated for 5 minute when all solid dissolved. The ss-TBD resin was removed by filtration and solvent was evaporated to yield a white foam (97% yield). Product was characterized by ES-MS as before.

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Brief introduction of 4-Methyl-1-piperazineacetic acid

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 11; Synthesis of Active Esters Of N-Methyl Piperazine Acetic Acid Via Oxalyl Chloride (Scheme B, FIG. 4B); To a suspension of N-methyl piperazine acetic acid (N-MPAA) (79 mg, 0.5 mmol) in DCM (25 mL) was added a solution of oxalyl chloride (4 mL, 0.8 mmol, 2.0 M solution in DCM) over 10 minute at room temperature. After another 30 minutes of reaction, solvent and excess reagent were removed under reduced pressure to give a white solid (23). A solution of NHS (57 mg, 0.5 mmol) in DCM (25 mL) was added to the solid followed by ss-TBD (390 mg, 1 mmol, 2.6 mmol/g). The resulting solution was sonicated for 5 minute when all solid dissolved. The ss-TBD resin was removed by filtration and solvent was evaporated to yield a white foam (97% yield). Product was characterized by ES-MS as before.

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 54699-92-2

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.

54699-92-2, Example 13; General Method For The Preparation Of Active Esters Of N-Substituted Piperazine Acetic Acid From Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 54699-92-2

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

54699-92-2, 4-Methyl-1-piperazineacetic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

54699-92-2, Example 13; General Method For The Preparation Of Active Esters Of N-Substituted Piperazine Acetic Acid From Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 4-Methyl-1-piperazineacetic acid

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.

54699-92-2, 36) 2-(4-methylpiperazin-1-yl)acetyl chloride [Show Image] Oxalil chloride (0.3 ml, 3.47 mmol) was added dropwise to a stirred solution of (4-Methyl-piperazin-1-yl)-acetic acid (500 mg, 3.16 mmol) 15 ml of dry THF and placed under inert atmosphere. Two drops of dimethylformammide were added. The reaction mixture was refluxed for 1 h, and the solvent removed under reduced pressure giving 440 mg (80%) (4-Methyl-piperazin-1-yl)-acetyl chloride as a yellow solid. 1H-NMR (DMSO, 400 MHz), delta (ppm): 3.20 (2H, s), 2.78 (8H, m), 2.60 (3H, s).

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; Universita Degli Studi Di Milano – Bicocca; UNIVERSITE DE GENEVE; UNIVERSITE CLAUDE BERNARD – LYON 1; EP2107054; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 4-Methyl-1-piperazineacetic acid

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 13; General Method For The Preparation Of Active Esters Of N-Substituted Piperazine Acetic Acid From Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 4-Methyl-1-piperazineacetic acid

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 11; Synthesis of Active Esters Of N-Methyl Piperazine Acetic Acid Via Oxalyl Chloride (Scheme B, FIG. 4B); To a suspension of N-methyl piperazine acetic acid (N-MPAA) (79 mg, 0.5 mmol) in DCM (25 mL) was added a solution of oxalyl chloride (4 mL, 0.8 mmol, 2.0 M solution in DCM) over 10 minute at room temperature. After another 30 minutes of reaction, solvent and excess reagent were removed under reduced pressure to give a white solid (23). A solution of NHS (57 mg, 0.5 mmol) in DCM (25 mL) was added to the solid followed by ss-TBD (390 mg, 1 mmol, 2.6 mmol/g). The resulting solution was sonicated for 5 minute when all solid dissolved. The ss-TBD resin was removed by filtration and solvent was evaporated to yield a white foam (97% yield). Product was characterized by ES-MS as before.

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 54699-92-2

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

54699-92-2, 4-Methyl-1-piperazineacetic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

54699-92-2, Example 13; General Method for the Preparation of Active Esters of N-Substituted Piperazine Acetic Acid from Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH2-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Applera Corporation.; US2005/148771; (2005); A1;; ; Patent; Applera Corporation.; US2005/148774; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 54699-92-2

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.

A solution of (1R,2R)-2-[[trans-2-[(1E,3E)-4-(4-cyano-2-fluorophenyl)-1,3-butadienyl]-1,3-dioxan-5-yl]thio]-1-(2,4-difluorophenyl)-1-[(1H-1,2,4-triazol-1-yl)methyl]propyl 2-(hydroxymethyl)benzoate (1.104 g, 1.63 mmol) obtained from Example 17-(4) in dichloromethane (25 ml) was cooled to 0C, and then 4-(N,N-dimethylamino)pyridine (299.1 mg, 2.45 mmol), 2-(4-methyl-1-piperazinyl)acetic acid (described in J. Med. Chem., 43, 1493 (2000); 387.3 mg, 2.45 mmol), and 1-ethyl-3-[3-(N,N-dimethylamino)propyl]carbodiimide (625.5 mg, 3.26 mmol) were added thereto. The reaction solution was stirred at room temperature for 4 hours, diluted with dichloromethane, and then the organic layer was washed successively with water and a saturated aqueous solution of sodium chloride. The solvent was evaporated under reduced pressure, and the residue was subjected to chromatography on a silica gel (40 g) column (eluent; ethyl acetate : methanol = 4 : 1) to give a mixture of the title target compound and 4-(N,N-dimethylamino)pyridine. The mixture was purified by recycle preparative HPLC [LC-908; Japan Analytical Industry Co., Ltd.; GPC column JAIGEL-1H (20 mm i.d. x 600 mm) and JAIGEL-2H (20 mm i.d. x 600 mm) connected in series for use; solvent, chloroform] to afford the title target compound (865.2 mg, 65% yield) as a colorless amorphous solid. NMR spectrum (400 MHz, CDCl3) delta ppm: 1.46 (3H, dd, J=7, 2 Hz), 2.29 (3H, s), 2.4-2.5 (4H, br s), 2.6-2.7 (4H, br s), 3.05 (1H, tt, J=12, 5 Hz), 3.31 (2H, s), 3.50 (1H, t, J=12 Hz), 3.53 (1H, t, J=12 Hz), 4.01 (1H, q, J=7 Hz), 4.12-4.21 (2H, m), 4 99 (1H, d, J=4 Hz), 5.45-5.55 (4H, m), 5.84 (1H, dd, J=15, 4 Hz), 6.57 (1H, dd, J=15, 10 Hz), 6.73 (1H, d, J=16 Hz), 6.93 (1H, dd, J=16, 10 Hz), 6.88-7.00 (2H, m), 7.34 (1H, dd, J=11, 1 Hz), 7.27-7.46 (3H, m), 7.53-7.60 (3H, m), 7.79 (1H, dd, J=8, 1 Hz), 7.90 (1H, s), 7.95 (1H, s) IR spectrum nu max KBr cm-1: 2230, 1726, 1503, 1275, 1257, 1051, 1140, 973 Mass spectrum m/z (FAB): 817 (M++1) Specific rotation [alpha]D25 +0.4 (c=0.99, CHCl3). A solution of (1R,2R)-2-[[trans-2-[(1E,3E)-4-(4-cyano-2-fluorophenyl)-1,3-butadienyl]-1,3-dioxan-5-yl]thio]-1-(2,4-difluorophenyl)-1-[(1H-1,2,4-triazol-1-yl)methyl]propyl 2-[[2-(4-methylpiperazin-1-yl)acetoxy]methyl]benzoate (280 mg, 0.343 mmol) obtained above in ethyl acetate (5 ml) was cooled to 0C, and hydrogen chloride (4N ethyl acetate solution; 95 mul, 0.38 mmol) was added thereto, and the mixture was stirred at 0C for 5 minutes. The solvent was evaporated under reduced pressure, and the residue was dried in vacuo to afford the mono hydrochloric acid salt of the title compound (298 mg, quantitative yield) as a pale yellow amorphous solid. NMR spectrum (400 MHz, CD3OD) delta ppm: 1.43 (3H, dd, J=7, 1 Hz), 2.87 (3H, s), 2.8-3.4 (8H, br), 3.04 (1H, tt, J=11, 5 Hz), 3.48 (1H, t, J=11 Hz), 3.53 (2H, s), 3.54 (1H, t, J=11 Hz), 4.06 (1H, q, J=7 Hz), 4.04-4.08 (2H, m), 4.17 (1H, ddd, J=11, 5, 2 Hz), 5.20 (1H, d, J=4 Hz), 5.46 (1H, d, J=14 Hz), 5.53 (1H, d, J=14 Hz), 5.58 (2H, s), 5.85 (1H, dd, J=15, 4 Hz), 6.57 (1H, dd, J=15, 10 Hz), 6.79 (1H, d, J=16 Hz), 7.01-7.11 (2H, m), 7.09 (1H, dd, J=16, 10 Hz), 7.46 (1H, td, J=8, 1 Hz), 7.50-7.61 (3H, m), 7.63 (1H, qd, J=7, 1 Hz), 7.78 (1H, t, J=8 Hz), 7.86 (1H, dd, J=7, 1 Hz), 7.95 (1H, s), 8.34 (1H, s) IR spectrum nu max KBr cm-1: 2230, 1726, 1503, 1274, 1257, 1140, 1050, 973 Mass spectrum m/z (FAB): 817 [M+(free base)+1] Specific rotation [alpha]D25 -1.9 (c=0.97, CHCl3). A solution of (1R,2R)-2-[[trans-2-[(1E,3E)-4-(4-cyano-2-fluorophenyl)-1,3-butadienyl]-1,3-dioxan-5-yl]thio]-1-(2,4-difluorophenyl)-1-[(1H-1,2,4-triazol-1-yl)methyl]propyl 2-[[2-(4-methylpiperazin-1-yl)acetoxy]methyl]benzoate (338.5 mg, 0.41 mmol) obtained above in ethyl acetate (5 ml) was cooled to 0C, and hydrogen chloride (4N ethyl acetate solution; 207 mul, 0.83 mmol) was added thereto, and the mixture was stirred at 0C for 5 minutes. The solvent was evaporated under reduced pressure, and the residue was dried in vacuo to afford the bis hydrochloric acid salt of the title compound (354 mg, quantitative yield) as a pale yellow amorphous solid. NMR spectrum (400 MHz, DMSO-d6) delta ppm: 1.35 (3H, dd, J=7, 2 Hz), 2.76 (3H, s), 2.82-2.92 (2H, br), 2.99 (1H, tt, J=11, 5 Hz), 3.06-3.16 (4H, br), 3.41 (2H, br d, J=15 Hz), 3.46 (1H, t, J=11 Hz), 3.47 (1H, t, J=11 Hz), 3.65 -3.75 (2H, br), 3.79 (1H, q, J=7 Hz), 3.96 (1H, ddd, J=11, 5, 2 Hz), 4.07 (1H, ddd, J=11, 5, 2 Hz), 5.05 (1H, d, J=5 Hz), 5.39 (1H, d, J=13 Hz), 5.40 (1H, d, J=14 Hz), 5.49 (1H, d, J=13 Hz), 5.56 (1H, d, J=14 Hz), 5.88 (1H, dd, J=15, 5 Hz), 6.56 (1H, dd, J=15, 11 Hz), 6.82 (1H, d, J=16 Hz), 7.16-7.20 (1H, m), 7.19 (1H, dd, J=16, 11 Hz), 7.31-7.37 (1H, m), 7.49-7.55 (1H, m), 7.55 (1H, td, J=9, 6 Hz), 7.60 (1H, d, J=7 Hz), 7.67-7.71 (2H, m), 7.84-7.89 (3H, m), 7.96 (1H, s), 8.44 (1H, s) Mass spectrum m/z (FAB): 817 [M+(free base)+1] Specific rotation [alpha]D25 -3.1 (c=1.87, CHCl3), 54699-92-2

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Sankyo Company, Limited; EP1362856; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 54699-92-2

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.

54699-92-2, Example 13; General Method For The Preparation Of Active Esters Of N-Substituted Piperazine Acetic Acid From Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10

54699-92-2 4-Methyl-1-piperazineacetic acid 2762732, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics