HRID596219

反应详情

EQUATION

反应方程式

HRID 596219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 2-hydroxyimino-2-phenylacetonitrile (14.6 g.) and dimethylaniline (13.2 g.) in a mixture of acetone (5 ml.) and benzene (80 ml.) was dropwise added to a solution of trichloromethyl chloroformate (phosgene dimer) (6.7 ml.) in benzene (30 ml.) under ice-cooling. The mixture was stirred for 6 hours at the same temperature and allowed to stand overnight. To the resultant mixture containing 2-chlorocarbonyloxyimino-2-phenylacetonitrile was dropwise added a mixture of tert-butyl alcohol (11.1 g.), pyridine (16.0 ml.) and benzene (20 ml.) under ice-cooling, and the mixture was stirred for 7 hours at room temperature and allowed to stand overnight. The reaction mixture was treated as described in the above Examples 2(A) to 2(F) to give 2-tert-butoxycarbonyloxyimino-2-phenylacetonitrile (17.0 g.), mp 84° to 86° C.

WORKUP

后处理

  1. temperaturecooling
  2. waitto stand overnight
  3. additionwas dropwise added
  4. temperaturecooling
  5. stirringthe mixture was stirred for 7 hours at room temperature
  6. waitto stand overnight
  7. additionThe reaction mixture was treated