HRID65821

反应详情

EQUATION

反应方程式

HRID 65821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 26.9 g of 4-(4-tert-butylphenethyloxy)aniline, 13 g of N-methoxy-N-methylcarbamyl chloride, 10 ml of pyridine and 300 ml of toluene is heated under reflux for 7 hours. Thereafter, water is added to dissolve pyridinium chloride, and the separated toluene layer is washed with dilute hydrochloric acid, thoroughly washed with water and dried over anhydrous sodium sulfate. The solvent is then removed under reduced pressure, and the crude crystals obtained are repeatedly recrystallized from ethanol to obtain 9.3 g of N'-[4-(4-tert-butylphenethyloxy)phenyl]-N-methoxy-N-methylurea as white needles, M.P. 14°-15° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 7 hours
  3. washthe separated toluene layer is washed with dilute hydrochloric acid
  4. washthoroughly washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent is then removed under reduced pressure
  7. customthe crude crystals obtained
  8. customare repeatedly recrystallized from ethanol