[OH-].[K+].[C:3]([C:6]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][C:21]([CH2:24][C:25]([O:27]CC)=[O:26])=[CH:20][C:19]=3[CH3:30])=[CH:14][CH:13]=2)[C:9]([CH3:31])=[N:8][C:7]=1[CH3:32])(=[O:5])[NH2:4].C(O)(=O)C>C(O)(C)(C)C.C(O)C>[C:3]([C:6]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][C:21]([CH2:24][C:25]([OH:27])=[O:26])=[CH:20][C:19]=3[CH3:30])=[CH:14][CH:13]=2)[C:9]([CH3:31])=[N:8][C:7]=1[CH3:32])(=[O:5])[NH2:4]Powdered potassium hydroxide (65.9 mg, 1.17 mmol) was added in one portion to ethyl 2-(4′-(6-carbamoyl-3,5-dimethylpyrazin-2-yl)-2-methylbiphenyl-4-yl)acetate (Intermediate 12-1; 79 mg, 0.20 mmol) in tert-butanol (2 mL) at 45° C. under nitrogen. The resulting solution was stirred at 45° C. for 1 hour. The mixture was treated with acetic acid (0.090 mL, 1.57 mmol) in ethanol (1 mL) and stirred at room temperature for 10 minutes. The mixture was then evaporated under vacuum to give an off white solid. This was triturated with water (10 mL), filtered off and washed with water (10 mL), before drying under vacuum to give desired product.
読み込み中…
