HRID1276506
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 89 mg of methyl ester (from Example 104, Step B) in 1.5 mL EtOH was added 1.0 mL of 0.5N NaOH. After 36 h the reaction was concentrated under vacuum. The residue was dissolved in 25 mL H2O and washed with 25 mL Et2O. After separating layers, the aqueous phase was acidified to pH 2 using 0.5N KHSO4. The aqueous phase was extracted with 3×25 mL of CH2Cl2. The combined extracts were dried over Na2SO4 and concentrated under vacuum to give 58 mg of a white foam which was taken on without further purification.
WORKUP
后处理
- concentrationAfter 36 h the reaction was concentrated under vacuum
- dissolutionThe residue was dissolved in 25 mL H2O
- washwashed with 25 mL Et2O
- customAfter separating layers
- extractionThe aqueous phase was extracted with 3×25 mL of CH2Cl2
- dry with materialThe combined extracts were dried over Na2SO4
- concentrationconcentrated under vacuum