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
Methanol (4 ml) and 1 ml of water were added to 1.277 g of methyl α-methylthio-α-[m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate. Furthermore, 350 mg of sodium hydroxide was added, and the mixture was heated under reflux for 2 hours. After cooling, 30 ml of water was added, and the mixture was washed twice with 10 ml of diethyl ether. To the aqueous layer was added about 6 ml of 3.5% hydrochloric acid to adjust its pH to 3. It was then extracted four times with 20 ml of diethyl ether. The organic layer was washed twice with 10 ml of water, dried over anhydrous sodium sulfate, and evaporated under reduced pressure to afford 1.199 g of α-methylthio-α-[m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionic acid as colorless crystals.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 2 hours
- temperatureAfter cooling
- washthe mixture was washed twice with 10 ml of diethyl ether
- additionTo the aqueous layer was added about 6 ml of 3.5% hydrochloric acid
- extractionIt was then extracted four times with 20 ml of diethyl ether
- washThe organic layer was washed twice with 10 ml of water
- dry with materialdried over anhydrous sodium sulfate
- customevaporated under reduced pressure