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
Methyl α-methylthio-α-(3-chloro-4-aminophenyl)propionate (380 mg) was dissolved in 4 ml of acetic acid, and an intimate mixture of 406 mg of zinc powder and 1.5 mg of anhydrous copper sulfate was added. The entire mixture was heated under reflux for 1 hour. Water (40 ml) and 15 ml of diethyl ether were added to the reaction mixture. The insoluble matter was separated by filtration, and then the organic layer was separated. Furthermore, the aqueous layer was extracted with 5 ml of diethyl ether. The organic layer and the extract were combined, washed with 15 ml of a saturated aqueous solution of sodium hydrogen carbonate, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford 299 mg of methyl α-(3-chloro-4-aminophenyl)propionate in a yield of 95.6% as a colorless oil.
WORKUP
后处理
- additionwas added
- temperatureThe entire mixture was heated
- temperatureunder reflux for 1 hour
- customThe insoluble matter was separated by filtration
- customthe organic layer was separated
- extractionFurthermore, the aqueous layer was extracted with 5 ml of diethyl ether
- washwashed with 15 ml of a saturated aqueous solution of sodium hydrogen carbonate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure