HRID1952854

反应详情

EQUATION

反应方程式

HRID 1952854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 106.3 g (0.489 mol) of ethyl 4,4-diethoxypentanoate and 80 ml (73.6 g, 0.99 mol) of ethyl formate was added dropwise to a vigorously stirred suspension of 12.7 g (0.55 gram atom) of sodium (shavings) in 300 ml of anhydrous benzene at 10-15° C. over 3 h. Stirring was continued for a further 3 h, and the reaction mixture was left to stand overnight. 250 ml of water were added with vigorous stirring, and this was continued for a further 15 min. The water layer was separated off, and the benzene layer was extracted with 70 ml of water. The combined aqueous extracts were acidified to pH 2 and extracted with ethyl acetate (5×50 ml), and the organic extracts were dried over calcium chloride.

WORKUP

后处理

  1. waitthe reaction mixture was left
  2. waitto stand overnight
  3. waitthis was continued for a further 15 min
  4. customThe water layer was separated off
  5. extractionthe benzene layer was extracted with 70 ml of water
  6. extractionextracted with ethyl acetate (5×50 ml)
  7. dry with materialthe organic extracts were dried over calcium chloride