反应详情

7 g of 2-[p-(phenylthio)phenoxy]ethylamine and 18.6 g of chlorothioformic acid S-ethyl ester are dissolved in 250 ml of acetone. 24 g of potassium carbonate are added to the solution and the mixture is heated under reflux for 6 hours. The mixture is then filtered, the residue is washed with acetone and the filtrate is evaporated in vacuo. The 13 g of residue are filtered through a 10-fold amount of silica gel with ether/cyclohexane (7:3). The first fractions yielded 10.2 g which, after recrystallization from ether/low boiling petroleum ether yields 6.3 g (76%) of 2-[p-(phenylthio)phenoxy]ethylthiocarbamic acid S-ethyl ester, m.p.--77°-79° C.

1. temperaturethe mixture is heated
2. temperatureunder reflux for 6 hours
3. filtrationThe mixture is then filtered
4. washthe residue is washed with acetone
5. customthe filtrate is evaporated in vacuo
6. filtrationThe 13 g of residue are filtered through a 10-fold amount of silica gel with ether/cyclohexane (7:3)
7. customThe first fractions yielded 10.2 g which
8. customafter recrystallization from ether/low