反应详情

To a solution containing 1.61 grams (0.004 moles) of 4-(2-chloro-4-phenylphenoxy)-2,5-dimethyl-3-chloroaniline prepared in Part B and 3 milliliters of toluene, which solution was warmed to 40° C.-50° C. and placed under an atmosphere of nitrogen, was added a solution containing 0.98 grams (0.005 moles) of 2-chlorobenzoyl isocyanate and 0.05 milliliters of toluene. The resulting mixture was then heated to a temperature of 60° C.-70° C, for a period of 0.5-1.0 hours. After cooling to ambient temperature, the reaction mixture was diluted with 4 milliliters of toluene and 2 milliliters of hexane. This mixture was then filtred to give a solid material. The solid material was washed once with a toluene-hexane mixture (1:2 volume ratio) and finally once with hexane and then dried overnight in a vaccum oven at 50° C. This afforded a tan powder material having a melting point of 198° C.-199° C. Elemental analysis of the tan powder indicated the following:

1. temperaturewas warmed to 40° C.-50° C.
2. additionwas added a solution
3. temperatureThe resulting mixture was then heated to a temperature of 60° C.-70° C, for a period of 0.5-1.0 hours
4. customto give a solid material
5. washThe solid material was washed once with a toluene-hexane mixture (1:2 volume ratio) and finally once with hexane
6. customdried overnight in a vaccum oven at 50° C
7. customThis afforded a tan powder material