反应详情

温度

60 °C

To a solution containing 1.55 grams (0.004 moles) of 3,5-dichloro-4-(2-phenylphenylmethoxy) aniline prepared in Part B and 5 milliliters of toluene, which solution was heated to a temperature of 60° C. and placed under an atmosphere of nitrogen, was added 0.98 grams (0.005 moles) of 2-chlorobenzoyl isocyanate. The resulting mixture was maintained at a temperature of 60° C. for a period of 0.5-1.0 hours. After cooling to ambient temperature, the reaction mixture was diluted with 1 milliliter of toluene. This mixture was then filtered to give a solid material. The solid material was washed once with toluene, once with a toluene-hexane mixture (1:1 volume ratio) and finally once with hexane and then dried overnight in a vacuum oven at 50° C. This afforded a white powder material having a melting point of 188.5° C.-192.0° C. Elemental analysis of the white powder indicated the following:

1. temperatureThe resulting mixture was maintained at a temperature of 60° C. for a period of 0.5-1.0 hours
2. temperatureAfter cooling to ambient temperature
3. filtrationThis mixture was then filtered
4. customto give a solid material
5. washThe solid material was washed once with toluene, once with a toluene-hexane mixture (1:1 volume ratio) and finally once with hexane
6. customdried overnight in a vacuum oven at 50° C
7. customThis afforded a white powder material