反应详情

To a solution of compound 1 (500 mg; 0.99 mmol) in methanol (10 ml) was added thiophene 3-carboxaldehyde (104 ul; 1.19 mmol) followed by acetic acid (0.1 ml; 1%) and sodium cyano borohydride (186.6 mg; 2.97 mmol). The reaction mixture was stirred overnight, then sodium hydroxide 2N was added and the mixture extracted with methylene chloride (3×). The combined methylene chloride extracts were dried over Na2SO4, filtered and concentrated under reduced pressure. Purification by reverse phase using 10%-30% CH3CN/H2O (TFA as the buffer) gave 258 mg of desired product (TFA salt).

1. extractionthe mixture extracted with methylene chloride (3×)
2. dry with materialThe combined methylene chloride extracts were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customPurification by reverse phase