HRID26360

反应详情

EQUATION

反应方程式

HRID 26360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.1 g (0.0254 moles) of salicylic aldehyde are dissolved in 30 ml of anhydrous toluene and 8.1 g (0.025 moles) of N-methyl-carbamic acid-pentachlorophenyl-ester are added under stirring at room temperature, whereafter 2.6 g (0.0257 moles) of triethylamine are added to the mixture under stirring. During the addition of the triethylamine an elevation of the temperature of about 2°-5° C. may be observed. The reaction mixture is stirred at 25°-30° C. for 2 hours, after about 1 hour the reaction mixture becomes clear. The unreacted active ester is filtered, the toluene is removed from the filtrate and the residual oily substance is recrystallized from a three-fold amount of diisopropylether. 2-methyl-carbamoyloxy-benzaldehyde is obtained. Mp.: 128°-132° C.

WORKUP

后处理

  1. additionare added to the mixture
  2. stirringThe reaction mixture is stirred at 25°-30° C. for 2 hours, after about 1 hour the reaction mixture
  3. filtrationThe unreacted active ester is filtered
  4. customthe toluene is removed from the filtrate
  5. customthe residual oily substance is recrystallized from a three-fold amount of diisopropylether