反应详情

温度

180 °C

An intimate mixture of 4-(N-methylamino)phenol acetate (7.3 g, 0.04 mole) and 6-bromo-2-(methylthio)benzoxazole (6.0 g, 0.025 mole) was prepared and heated on an oil bath to a temperature of 180° C. The mixture was heated at this temperature for a period of 4 hours during which time acetic acid distilled from the mixture and methyl mercaptan was evolved and was trapped in aqueous sodium hydroxide. The mixture was cooled to form a solid and the solid was extracted with hot toluene (4×100 ml). The toluene solution was filtered hot and the solvent removed by distillation to give a brown solid. The solid was recrystallised from toluene to give the title compound as a grey solid (3.5 g), mp 195° C.

1. customwas prepared
2. distillationdistilled from the mixture and methyl mercaptan
3. temperatureThe mixture was cooled
4. customto form a solid
5. extractionthe solid was extracted with hot toluene (4×100 ml)
6. filtrationThe toluene solution was filtered hot
7. customthe solvent removed by distillation
8. customto give a brown solid
9. customThe solid was recrystallised from toluene