反应详情

51.0 g (0.254 m), 5-chloro-2-mercaptobenzothiazole, 22.8 g (0.304 m) chloroacetonitrile and 30.7 g triethylamine are dissolved in 600 ml of toluene and the solution is heated to reflux for 3 hr, then allowed to cool to room temperature. The toluene solution is washed with water, dried over anhydrous magnesium sulfate and treated with Darco. After the solvent is removed, the residual solid is recrystallized from 300 ml. benzene. The recovered material is recrystallized from cyclohexane. A total yield of 52 g (86%) is obtained. The recrystallized sample has a melting point of 96°-7° C.

1. temperaturethe solution is heated
2. temperatureto reflux for 3 hr
3. washThe toluene solution is washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. additiontreated with Darco
6. customAfter the solvent is removed
7. customthe residual solid is recrystallized from 300 ml
8. customThe recovered material is recrystallized from cyclohexane
9. customA total yield of 52 g (86%) is obtained