反应详情

To a solution of the intermediate from step A (2.7 g, 10 mmol) in 10:1 MeOH:H2O (60 mL) was added potassium carbonate (2.76 g, 20 mmol). The reaction was stirred at room temperature for 15 minutes after which the mixture was poured into a pH 7-phosphate buffer and extracted with methylene chloride (3×). The combined organic layers were then dried over anhydrous MgSO4, filtered and concentrated in vacuo. The resulting oil was used without further purification. 1H NMR (CDCl3, 500 MHz): 7.8 (d, J=1.9 Hz, 1H), 7.5 (m, 2H), 3.48 (s, 1H).

1. extractionextracted with methylene chloride (3×)
2. dry with materialThe combined organic layers were then dried over anhydrous MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe resulting oil was used without further purification