HRID603915
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Ethyl ({[2-(1,3-benzodioxol-5-yl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetate (Method 12) (14.2 g, 0.039 mol) was dissolved in THP (300 mL) and cooled to 0° C. LiOH (4.87 g, 0.12 mol) in water (100 mL) was added, and the mixture was given room temperature and stirred for 19 hours. The solvents were evaporated, the crude product was added water and extracted with diethyl ether. The aqueous layer was added 1M HCl until pH=3 and extracted twice with CH2Cl2. The combined CH2Cl2 layers were dried (Na2SO4) and concentrated under reduced pressure to afford the desired product.
WORKUP
后处理
- customwas given room temperature
- customThe solvents were evaporated
- additionthe crude product was added water
- extractionextracted with diethyl ether
- additionThe aqueous layer was added 1M HCl until pH=3
- extractionextracted twice with CH2Cl2
- dry with materialThe combined CH2Cl2 layers were dried (Na2SO4)
- concentrationconcentrated under reduced pressure