HRID442284

反应详情

EQUATION

反应方程式

HRID 442284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 27.4 g of 3,4-dichloroaniline in 140 ml of isopropyl ether was added slowly to 9 g of methyl isocyanate in 100 ml of isopropyl ether and the mixture was refluxed for 2 hours and was then cooled to 0° C. The precipitate formed was recovered by vacuum filtration and was washed with isopropyl ether. The mother liquors were concentrated to obtain a second crop. The two combined crops weighing 19.5 g and melting at 156° C. were crystallized from ethyl acetate to obtain N-methyl-N'-(3,4-dichlorophenyl)-urea melting at 160° C., identical to the product described by Onley et al., J. Ass. Off. Anal. Chem., Vol. 52 (1969), p. 545.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. customThe precipitate formed
  3. filtrationwas recovered by vacuum filtration
  4. washwas washed with isopropyl ether
  5. concentrationThe mother liquors were concentrated
  6. customto obtain a second crop
  7. customwere crystallized from ethyl acetate