反应详情

To a solution of compound 1 (0.99 mmol) in methylene chloride (10 ml) was added 2-thiophenecarboxaldehyde (190 ul; 1.98 mmol) followed by acetic acid (0.1 ml; 1%). The mixture was stirred 30 minutes then sodium triacetoxyborohydride (0.63 g; 2.97 mmol) was added and the reaction mixture stirred overnight. The reaction mixture was neutralized with sodium hydroxide 2N and 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 115 mg of desired product (TFA salt).

1. stirringthe reaction mixture stirred overnight
2. extractionextracted with methylene chloride (3×)
3. dry with materialThe combined methylene chloride extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customPurification by reverse phase