HRID2291844

反应详情

EQUATION

反应方程式

HRID 2291844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl (2,2-dimethoxyethyl)malonate (115.0 g, 0.46 mol) was added to a suspension of lithium aluminum hydride (38.0 g, 1.00 mol) in 400 ml of dry ether at a rate to maintain a gentle reflux. After stirring for 15 min. 40 ml of water, 40 ml of 15% aqueous NaOH, and 120 ml of water were added and stirring was continued until a white suspension was obtained. The inorganic salts were filtered off and extracted with several 200 ml portions of tetrahydrofuran (THF). The combined organic extracts were evaporated and distilled twice in vacuum to yield 50.23 g (66.5%) of the title compound. B.p. 116°-125° (0.02 mm Hg).

WORKUP

后处理

  1. temperatureto maintain a gentle reflux
  2. stirringstirring
  3. customwas obtained
  4. filtrationThe inorganic salts were filtered off
  5. extractionextracted with several 200 ml portions of tetrahydrofuran (THF)
  6. customThe combined organic extracts were evaporated
  7. distillationdistilled twice in vacuum