反应详情

In 800 ml of pyridine were dissolved 275 ml of carbon disulfide and 93 ml of triethylamine. To the solution was added 125 g of 4-bromo-2-methylaniline. The mixture was stirred at room temperature overnight. Thereto was added 138.5 g of 1,3-dicyclohexylcarbodiimide (DCC). The mixture was stirred overnight. Pyridine was removed by distillation. To the residue was added n-hexane. The resulting precipitate (DC-thiourea) was removed by filtration. The filtrate was concentrated and the residue was purified by a silica gel column chromatography (eluant: n-hexane) to obtain 138 g of 4-bromo-2-methylphenyl isothiocyanate.

1. stirringThe mixture was stirred overnight
2. customPyridine was removed by distillation
3. additionTo the residue was added n-hexane
4. customThe resulting precipitate (DC-thiourea) was removed by filtration
5. concentrationThe filtrate was concentrated
6. customthe residue was purified by a silica gel column chromatography (eluant: n-hexane)