HRID1940480

反应详情

EQUATION

反应方程式

HRID 1940480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of diethyl cis-1,2-cyclopropanedicarboxylate (53.0 g, 284.6 mmol) and sodium hydroxide (32.4 g, 809.1 mmol) in water (200 mL) was heated at reflux for 5 h. The mixture was then allowed to stir at room temperature overnight. The ethanol formed was evaporated under reduced pressure and the remaining aqueous solution was acidified with a slight excess of concentrated aqueous HCl (74.8 mL, 92.8 mmol). The mixture was evaporated to dryness under reduced pressure, and the residue was washed with hot ethyl acetate (3 times with 200 mL). The ethyl acetate layer was separated, dried (MgSO4) and evaporated to dryness under reduced pressure to give 35.5 g of the title compound of Step B as a white solid (96% yield); m.p. 122°-124° C. IR (mineral oil, cm-1), 1691.0 (C=O); 2600-3100, broad (OH).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 5 h
  3. customwas evaporated under reduced pressure
  4. customThe mixture was evaporated to dryness under reduced pressure
  5. washthe residue was washed with hot ethyl acetate (3 times with 200 mL)
  6. customThe ethyl acetate layer was separated
  7. dry with materialdried (MgSO4)
  8. customevaporated to dryness under reduced pressure