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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
As in Example 1, bis(2-cyanoethoxy)ethane was prepared by the addition of 623 g (11.73 moles) of acrylonitrile to 310 g (5.0 moles) of ethylene glycol containing 1.0 g of anhydrous lithium hydroxide at 55°-60° C. over a period of 90 min. The reaction was permitted to stir an additional 2 hr at 50° C. The reaction contents were cooled to 25° C. and 88.0 g (2.75 moles) of methanol was added over a period of 1 hr while maintaining the temperature between 25°-30° C. The mixture was allowed to stir an additional 12 hr at room temperature. Analysis by NMR revealed the crude product mixture to be 79.7 wt % of bis(2-cyanoethoxy)ethane, 17.4 wt % methoxypropionitrile, 1.78 wt % methanol, 0.72 wt % of 2-cyanoethoxyethanol, and 0.33 wt % acrylonitrile.
WORKUP
后处理
- customThe reaction contents
- temperaturewere cooled to 25° C.
- temperaturewhile maintaining the temperature between 25°-30° C
- stirringto stir an additional 12 hr at room temperature