反应详情

To a solution of 4-((3,4-dichlorophenyl)(hydroxy)methyl)-3-methoxybenzamide (Preparation 156, 142 mg, 0.435 mmol) in DCM (5 mL) was added TFA (0.065 mL, 0.870 mmol) followed by triethylsilane (0.083 mL, 0.522 mmol) and the reaction stirred at room temperature for 72 hours. Further TFA (0.065 mL, 0.870 mmol) and triethylsilane (0.083 mL, 0.522 mmol) were added and the reaction stirred for a further 24 hours. The reaction was partitioned between saturated aq. NH4Cl (20 mL), and EtOAc (20 mL). The layers were separated and the aqueous was extracted with EtOAc (2×20 mL). The combined organics were washed with brine (20 mL), dried over MgSO4, filtered and the solvent removed in vacuo to give a white solid (165 mg, 100%). The material was used as crude in the next reaction without further purification.

1. stirringthe reaction stirred for a further 24 hours
2. customThe reaction was partitioned between saturated aq. NH4Cl (20 mL), and EtOAc (20 mL)
3. customThe layers were separated
4. extractionthe aqueous was extracted with EtOAc (2×20 mL)
5. washThe combined organics were washed with brine (20 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customthe solvent removed in vacuo