普瑞巴林二酸杂质

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of lithium hydroxide monohydrate (26 mg, 0.61 mmol) in water (250 μl) was added to a stirred solution of (2R) 2-isobutylsuccinic acid 1-methyl ester (100 mg, 0.53 mmol) in 1,4-dioxane (500 μl). The mixture was stirred for 2 hours then lithium hydroxide monohydrate (26 mg, 0.61 mmol) was added and stirring continued for 24 hours. The majority of solvents were removed by distillation in vacuo then the residue was dissolved in water (5 ml) and acidified using hydrochloric acid (1M) to pH=1. The product was extracted into dichloromethane (5×5 ml), dried (Na2SO4) and the solvent removed in vacuo to obtain (2R) 2-isobutylsuccinic acid (49 mg, 53%) as a solid. HPLC-MS (single UV peak with Rt=6.223 mins, 197.1 [M+Na]+). stirring continued for 24 hours The majority of solvents were removed by distillation in vacuo the residue was dissolved in water (5 ml) The product was extracted into dichloromethane (5×5 ml) dried (Na2SO4) the solvent removed in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of lithium hydroxide monohydrate (26 mg, 0.61 mmol) in water (250 μl) was added to a stirred solution of (2R) 2-isobutylsuccinic acid 1-methyl ester (100 mg, 0.53 mmol) in 1,4-dioxane (500 μl). The mixture was stirred for 2 hours then lithium hydroxide monohydrate (26 mg, 0.61 mmol) was added and stirring continued for 24 hours. The majority of solvents were removed by distillation in vacuo then the residue was dissolved in water (5 ml) and acidified using hydrochloric acid (1M) to pH=1. The product was extracted into dichloromethane (5×5 ml), dried (Na2SO4) and the solvent removed in vacuo to obtain (2R) 2-isobutylsuccinic acid (49 mg, 53%) as a solid. HPLC-MS (single UV peak with Rt=6.223 mins, 197.1 [M+Na]+). stirring continued for 24 hours The majority of solvents were removed by distillation in vacuo the residue was dissolved in water (5 ml) The product was extracted into dichloromethane (5×5 ml) dried (Na2SO4) the solvent removed in vacuo

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of lithium hydroxide monohydrate (26 mg, 0.61 mmol) in water (250 μl) was added to a stirred solution of (2R) 2-isobutylsuccinic acid 1-methyl ester (100 mg, 0.53 mmol) in 1,4-dioxane (500 μl). The mixture was stirred for 2 hours then lithium hydroxide monohydrate (26 mg, 0.61 mmol) was added and stirring continued for 24 hours. The majority of solvents were removed by distillation in vacuo then the residue was dissolved in water (5 ml) and acidified using hydrochloric acid (1M) to pH=1. The product was extracted into dichloromethane (5×5 ml), dried (Na2SO4) and the solvent removed in vacuo to obtain (2R) 2-isobutylsuccinic acid (49 mg, 53%) as a solid. HPLC-MS (single UV peak with Rt=6.223 mins, 197.1 [M+Na]+). stirring continued for 24 hours The majority of solvents were removed by distillation in vacuo the residue was dissolved in water (5 ml) The product was extracted into dichloromethane (5×5 ml) dried (Na2SO4) the solvent removed in vacuo

反应条件: temp:0.00; pressure:0.00; stir: