反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customequipped with a thermometer
- temperaturereflux condenser, tap funnel and magnetic stirrer
- temperatureSubsequently, the mixture is cooled to 10° to 15° C. by means
- additionis added drop-wise at such a rate that the temperature of the reaction mixture
- temperatureSubsequently, the mixture is heated to 40° to 50° C. for 1 hour
- additionwere added, under intensive stirring
- extractionis extracted with ether
- customas explained in Preparation Example 1