反应详情

A suspension of 21 (9.8 g, 22 mmol) in sodium methoxide (28% in MeOH; 400 g) was heated at reflux temperature for 9 hours. The resulting solution was poured on ice (300 ml) and extracted with CH2Cl2 (150 ml) three times. The combined extracts were dried over sodium sulfate (Na2SO4) and concentrated. The clude was purified by recrystallization from ethanol (EtOH) to give 22 (1:4 mixture at 6-position ; 8.4 9, 19 mmol, 87%).

1. temperaturewas heated
2. temperatureat reflux temperature for 9 hours
3. additionThe resulting solution was poured on ice (300 ml)
4. extractionextracted with CH2Cl2 (150 ml) three times
5. dry with materialThe combined extracts were dried over sodium sulfate (Na2SO4)
6. concentrationconcentrated
7. customThe clude was purified by recrystallization from ethanol (EtOH)