HRID862119
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 22 (6.5 g, 15 mmol) in 6N-HCl aq (100 ml) was heated at reflux for 10 hours. The resulting solution of sodium hydroxide (NaOH) (24 g) in water (100 ml) and extracted with CH2Cl2 (100 ml) four times. The combined extracts were dried over Na2SO4 and concentrated. The clude was purified by recrystallization from EtOH to give 23 (1:1 mixture at 6-position; 10 mmol, 68%).
WORKUP
后处理
- temperatureat reflux for 10 hours
- extractionThe resulting solution of sodium hydroxide (NaOH) (24 g) in water (100 ml) and extracted with CH2Cl2 (100 ml) four times
- dry with materialThe combined extracts were dried over Na2SO4
- concentrationconcentrated
- customThe clude was purified by recrystallization from EtOH