Реакция #5727

Уравнение реакции

2,6-dichlorobenzoylisocyanate

p-chloroaniline-acetonitrile

→

N-(2,6-dichlorobenzoyl)-N'-(cyanomethyl)-N'-(p-chlorophenyl)-urea

Выход 80.0%

Растворители

benzene

Условия реакции

Обработка

1. 1
   ДругоеAfter some time a substance crystallizes out
2. 2
   Промывкаwashed with benzene
3. 3
   ДругоеAfter drying the weight
4. 4
   Другоеbeing 185° C. with spontaneous decomposition on the Kofler
5. 5
   Температураheating bench
6. 6
   Другоеit may be recrystallized from 250 ml of benzene with a yield of 80%

Методика

16.0 g of 2,6-dichlorobenzoylisocyanate are added in small portions to a solution of 11.66 g of p-chloroaniline-acetonitrile in 100 ml of dry benzene with moderate cooling. After some time a substance crystallizes out, which after about 12 hours is drawn off and washed with benzene. After drying the weight is 25.25 g, i.e. 93.7% the melting point being 185° C. with spontaneous decomposition on the Kofler heating bench. Thin-layer chromatography (solvent either ethylacetate or chloroform) shows that the substance is pure, however, if desired, it may be recrystallized from 250 ml of benzene with a yield of 80%.

Источник