反应详情

A solution of 3-benzoxazol-2-yl-4-trifluoromethoxyphenylamine (210 mg, 0.71 mmol) in 5 mL of dry toluene was stirred while 1.15 mL of 3.1N hydrochloric acid in ethyl acetate was added. The precipitate was concentrated by evaporation. Another 5 mL of toluene was added followed by evaporation. This procedure was repeated 3 times to remove excess of hydrochloric acid. The amine hydrochloride was dissolved in 5 mL of toluene and trichloromethyl chloroformate (0.853 mL, 7.1 mmol) was added. The mixture was refluxed overnight under a nitrogen atmosphere, evaporated at 70° C. followed by stripping with dry toluene. 2-(5-Isocyanato-2-trifluoromethoxyphenyl)benzoxazole (160 mg, 70%) was obtained as crystals and used immediately to synthesize the title compound.

1. additionwas added
2. concentrationThe precipitate was concentrated by evaporation
3. additionAnother 5 mL of toluene was added
4. customfollowed by evaporation
5. customto remove excess of hydrochloric acid
6. dissolutionThe amine hydrochloride was dissolved in 5 mL of toluene
7. temperatureThe mixture was refluxed overnight under a nitrogen atmosphere
8. customevaporated at 70° C.