HRID27997

反应详情

EQUATION

反应方程式

HRID 27997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
145 °C

PROCEDURE

实验过程

A glass pressure vessel was charged with 5.5 grams (0.02 mole) 1-methyl-3-(3-trichloromethyl-1,2,4-thiadiazol-5-yl)urea, 3.2 grams (0.02 mole) benzoyl isocyanate and 50 milliliters benzene. A magnetic stirring bar was added and the vessel sealed. The stirred reaction mixture was heated at 145° C. for 1.5 hours and then allowed to cool to room temperature where 4.5 grams of starting urea precipitates. The urea was removed by filtration and the filtrate concentrated in vacuo to leave 3.0 grams of residue. Extraction of the residue with hot cyclohexane, followed by cooling the extract yielded 0.2 grams (11% selectivity) of pure product; m.p. 70° C.

WORKUP

后处理

  1. additionA magnetic stirring bar was added
  2. customthe vessel sealed
  3. customThe stirred reaction mixture
  4. customprecipitates
  5. customThe urea was removed by filtration
  6. concentrationthe filtrate concentrated in vacuo