HRID27293

反应详情

EQUATION

反应方程式

HRID 27293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.0 g (0.031 mole) of 3-ethyl-1,1-dicarbethoxycyclobutane (prepared in 1C) dissolved in 7 ml of absolute ethanol was prepared. To this solution there was added 6.87 g (0.123 mole) of potassium hydroxide dissolved in 76 ml of absolute ethanol and the mixture was heated to reflux with stirring for 1.5 hr. The mixture was then filtered and the filter cake was washed with 10 ml of absolute ethanol and 75 ml of ether. The resulting filter cake was dissolved in 30 ml of ice water and acidified with 36 ml of 50% aqueous sulfuric acid. The resulting mixture was cooled, filtered and dried to yield 4.5 g of the title compound having the following physical characteristics:

WORKUP

后处理

  1. customwas prepared
  2. temperaturethe mixture was heated
  3. temperatureto reflux
  4. filtrationThe mixture was then filtered
  5. washthe filter cake was washed with 10 ml of absolute ethanol and 75 ml of ether
  6. filtrationThe resulting filter cake
  7. dissolutionwas dissolved in 30 ml of ice water
  8. temperatureThe resulting mixture was cooled
  9. filtrationfiltered
  10. customdried