HRID648770

反应详情

EQUATION

反应方程式

HRID 648770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

With vigorous stirring, a solution of 12 g of NaOH in 20 ml of water is added to a solution of 27 g (0.08 mole) of α-(4-acetoxybenzenesulfonyloxyimino)thienylacetonitrile (3c) in 125 ml of tetrahydrofuran. After 1 hour, the reaction mixture is acidified with 20% hydrochloric acid and, after the addition of water and diethyl ether, the phases are separated. The aqueous phase is extracted with ether, the combined organic phases are dried over MgSO4, and the solvent is distilled off. The residual crude product is recrystallised from toluene, affording 17 g of beige-coloured crystals which melt at 151°-152° C.

WORKUP

后处理

  1. customthe phases are separated
  2. extractionThe aqueous phase is extracted with ether
  3. dry with materialthe combined organic phases are dried over MgSO4
  4. distillationthe solvent is distilled off
  5. customThe residual crude product is recrystallised from toluene