HRID65820

反应详情

EQUATION

反应方程式

HRID 65820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a solution of 10.6 g of 4-(4-isopropylphenethyloxy)phenylcarbamyl chloride in 200 ml of toluene are added 4 ml of pyridine and a solution of 2.5 g of N,O-dimethylhydroxylamine in 50 ml of toluene at a temperature below 20° C. The mixture is heated under reflux for 4 hours. The reaction mixture is then poured into ice water, and the separated organic layer is washed with dilute hydrochloric acid, thoroughly washed with water and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure, and the crude crystals are recrystallized from ethanol to obtain 4.8 g of N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea as white needles, M.P. 81°-82° C.

WORKUP

后处理

  1. customat a temperature below 20° C
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 4 hours
  4. washthe separated organic layer is washed with dilute hydrochloric acid
  5. washthoroughly washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent is removed under reduced pressure
  8. customthe crude crystals are recrystallized from ethanol