HRID35268

反应详情

EQUATION

反应方程式

HRID 35268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium hydroxide (2.15 g, 54 mmol) in water (15 ml) was added dropwise to a stirred solution of diethyl 1,1-cyclopropanedicarboxylate (10 g, 54 mmol) in ethanol (30 ml) while the temperature was maintained below 25° C. After the completion of the addition, the resulting mixture was stirred at room temperature for 60 hours. Most of ethanol was removed by evaporation in vacuo and the residue was diluted with brine, acidified with 6N hydrochloric acid and extracted with diethyl ether. The extract was dried over magnesium sulfate, filtered and concentrated. The residue was purified by distillation to give the title compound (bp 66°-9° C./0.15 mm) as a viscous oil.

WORKUP

后处理

  1. temperaturewas maintained below 25° C
  2. additionAfter the completion of the addition
  3. customMost of ethanol was removed by evaporation in vacuo
  4. additionthe residue was diluted with brine
  5. extractionextracted with diethyl ether
  6. dry with materialThe extract was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. distillationThe residue was purified by distillation