反应详情

To a mixture of 2-(2,5-dihydro-pyrrole-1-carbonyl)-1H-imidazole-4-carboxylic acid ethyl ester (100 mg, 0.43 mmol) and (2,3-difluoro-phenyl)acetic acid (75 mg, 0.44 mmol) in anhydrous THF (5 mL) was added LDMS (1.0M in THF, 1.5 mL, 1.5 mmol) at −78° C. After addition of LDMS, the dry-ice bath was removed and the reaction was stirred at ambient temperature for 6 hours. To this reaction mixture was added 1 mL of sat. NH4Cl solution and EtOAc then the organic layer was separated and dried over MgSO4. After removal of solvent, the residue was washed with water to afford the title compound as a yellow solid. This crude product was used directly for the next step without further purification. MS (ES+): m/e=318.2 (M+H); Rt=3.21 minutes.

1. additionAfter addition of LDMS
2. customthe dry-ice bath was removed
3. additionTo this reaction mixture was added 1 mL of sat. NH4Cl solution and EtOAc
4. customthe organic layer was separated
5. dry with materialdried over MgSO4
6. customAfter removal of solvent
7. washthe residue was washed with water