HRID553628
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 potassium hydroxide (1.8 g, 338 mmol) and 3-benzyloxy-2,2-dimethyl-propionic acid methyl ester in ethanol (50.0 mL) is refluxed for 24 h. The solvent is removed under reduced pressure, the crude is diluted with water and extracted with ethyl acetate. The water phase is acidified with 1N aq. HCl (pH ˜2-3) and extracted with ethyl acetate. The combined organic layers are washed with water and brine; the organic phase is dried over Na2SO4, filtered and concentrated under reduced pressure to afford 2.5 g of 3-benzyloxy-2,2-dimethyl-propionic acid as a brown solid that is used in the next step without any further purification. Yield: 32%, over two steps; m/z 209 [M+H].
WORKUP
后处理
- customThe solvent is removed under reduced pressure
- additionthe crude is diluted with water
- extractionextracted with ethyl acetate
- extractionextracted with ethyl acetate
- washThe combined organic layers are washed with water and brine
- dry with materialthe organic phase is dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure