反应详情

p-Bromophenyl isocyanate (20 g., 0.10 mole) was added in portions to a solution of 27.6 g. (0.10 mole) of 2-amino-6,7-dichloro-4-thiocyanatobenzothiazole in 300 ml. of dimethylformamide. The solution was heated at 100° with stirring for 41/2 hours and cooled at 0° overnight. The solid was collected by filtration. The filtrate was poured into ice water and the solid was collected by filtration. The combined solids were recrystallized from a methanol-dimethylformamide-water mixture to give 22 g. (50%) of product. Recrystallization from ethanol gave an analytical sample, m.p. 243°-245° .

1. temperatureThe solution was heated at 100°
2. temperaturecooled at 0° overnight
3. filtrationThe solid was collected by filtration
4. additionThe filtrate was poured into ice water
5. filtrationthe solid was collected by filtration
6. customThe combined solids were recrystallized from a methanol-dimethylformamide-water mixture
7. customto give 22 g
8. customRecrystallization from ethanol
9. customgave an analytical sample, m.p. 243°-245°