HRID1939854

反应详情

EQUATION

反应方程式

HRID 1939854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

48.2 g 4-amino butyraldehyde diethyl acetal are dissolved in 48.2 g water-free pyridine at 20 ° C. under stirring in a three-necked flask, equipped with a thermometer, reflux condenser, tap funnel and magnetic stirrer. Subsequently, the mixture is cooled to 10° to 15° C. by means of external cooling and at these temperatures 34,6 g methane sulfochloride is added drop-wise at such a rate that the temperature of the reaction mixture does not rise beyond the given range. Subsequently, the mixture is heated to 40° to 50° C. for 1 hour and then stirred into 300 g ice water, to which 20 g of concentrated hydrochloric acid were added, under intensive stirring. The resulting substance is a two-phase, yellow-brown mixture, which is extracted with ether and further processed as explained in Preparation Example 1. Yield: 88% based on the amino acetal used.

WORKUP

后处理

  1. customequipped with a thermometer
  2. temperaturereflux condenser, tap funnel and magnetic stirrer
  3. temperatureSubsequently, the mixture is cooled to 10° to 15° C. by means
  4. additionis added drop-wise at such a rate that the temperature of the reaction mixture
  5. temperatureSubsequently, the mixture is heated to 40° to 50° C. for 1 hour
  6. additionwere added, under intensive stirring
  7. extractionis extracted with ether
  8. customas explained in Preparation Example 1