HRID1925708
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
To a solution of 55 (0.817 g; 2.31 mmol) in methanol (4.5 mL) was added aqueous sodium hydroxide (9.2 mL; 1N). After the reaction was complete, the mixture was partitioned between diethyl ether and water; the organic layer was separated and set aside. The aqueous layer was acidified with excess aqueous hydrochloric acid (2N) and extracted with ethyl acetate (2×). The diethyl ether and ethyl acetate organic layers were combined, dried over sodium sulfate, decanted, and concentrated under reduced pressure. The resulting residue yielded the desired product a white solid from a mixture of hexanes and dichloromethane (0.54 g).
WORKUP
后处理
- customthe mixture was partitioned between diethyl ether and water
- customthe organic layer was separated
- extractionextracted with ethyl acetate (2×)
- dry with materialdried over sodium sulfate
- customdecanted
- concentrationconcentrated under reduced pressure