反应详情

100 g of 2-(1,3-benzodioxol-5-yl)ethanethiol and 75.1 g of bromoacetic acid were dissolved in 1 l of ethanol. A solution of 44 g of sodium hydroxide in 125 ml of water and then 2 l of ethanol were added thereto. The mixture was heated under reflux for 3 h. The reaction mixture was concentrated under reduced pressure. 2.5 l of water was added thereto. The mixture was made alkaline with a 1N sodium hydroxide solution, washed with 35% hydrochloric acid, extracted with ethyl acetate, washed with water four times and dried over sodium sulfate. The solvent was distilled off under reduced pressure to obtain 121 g of [{2-(1,3-benzodioxol-5-yl)ethyl}thio]acetic acid in the form of a faint yellow oil.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 h
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. addition2.5 l of water was added
5. washwashed with 35% hydrochloric acid
6. extractionextracted with ethyl acetate
7. washwashed with water four times
8. dry with materialdried over sodium sulfate
9. distillationThe solvent was distilled off under reduced pressure