HRID1283760

反应详情

EQUATION

反应方程式

HRID 1283760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 2-chlorocarbonyloxyimino-2-cyanoacetate (0.05 mol) prepared as in Example 11 (1), a solution of 2,4,5-trichlorophenol (9.9 g) and pyridine (3.9 g) in benzene (50 ml) is dropwise added under cooling with icewater. The resulting mixture is stirred for 1 hour and allowed to stand over night. The reaction mixture is washed with water, dried and concentrated. The residue is admixed with petroleum ether and filtered to collect crystals, which is dried and recrystallized from a benzene-petroleum ether mixture to give ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate (12.0 g). M.P. 101 to 103°C.

WORKUP

后处理

  1. temperatureunder cooling with icewater
  2. waitto stand over night
  3. washThe reaction mixture is washed with water
  4. customdried
  5. concentrationconcentrated
  6. filtrationfiltered
  7. customto collect crystals, which
  8. customis dried
  9. customrecrystallized from a benzene-petroleum ether mixture