HRID582726

反应详情

EQUATION

反应方程式

HRID 582726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
27.5 °C

PROCEDURE

实验过程

A mixture of 60 g of ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate and 300 ml of 1 N sodium hydroxide was stirred at 25-30° C. After 2.5 hours, concentrated hydrochloric acid was added to adjust the pH to 0.8-1.2. The resulting solution was extracted with ethyl acetate. The extracts were dried over magnesium sulfate, filtered, and concentrated to give 49.1 g (98%) of the crude material. Recrystallization from 100 ml of ethyl acetate gave the title compound, mp 123.5-128° C. FDMS: m/z =140 (M+) Analysis calculated for C7H8O3 : C, 60.00; H, 5.75. Found: C, 60.14; H, 5.79.

WORKUP

后处理

  1. extractionThe resulting solution was extracted with ethyl acetate
  2. dry with materialThe extracts were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give 49.1 g (98%) of the crude material
  6. customRecrystallization from 100 ml of ethyl acetate