反应详情

To a solution of the product of Step 1 (79.6 mg, 0.157 mmol) in methanol (4 mL) and ethyl acetate (2 mL), was added 10% palladium on carbon (18 mg) and the reaction mixture was stirred under an atmosphere of hydrogen (balloon) overnight. LC/MS analysis showed the reaction was not quite complete so an additional 10% palladium on carbon (10 mg) was added and the reaction mixture was stirred under an atmosphere of hydrogen (balloon) for an additional 6 hours. The reaction mixture was filtered through a microfilter and the collected solid was washed well with methanol. The filtrate was concentrated under vacuum and azeotroped with toluene to afford the title compound as a light brown oil which was used directly in the next step without purification

1. additionwas added
2. stirringthe reaction mixture was stirred under an atmosphere of hydrogen (balloon) for an additional 6 hours
3. filtrationThe reaction mixture was filtered through a microfilter
4. washthe collected solid was washed well with methanol
5. concentrationThe filtrate was concentrated under vacuum
6. customazeotroped with toluene