HRID372039

反应详情

EQUATION

反应方程式

HRID 372039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 10.2 g of 2,2-diethoxy acetaldehyde, 27.8 g of methyl triphenylphosphoranylidene-acetate and 130 ml of benzene is refluxed for 15 hours and evaporated. The residue is triturated with diethyl ether, filtered and the filtrate evaporated. The residue is allowed to stand overnight in the refrigerator, triturated with the minimum amount of diethyl ether, the suspension filtered, the filtrate evaporated, the residue distilled and the fraction boiling at 50°-54°/0.1 mm Hg collected, to yield the 4,4-diethoxy-crotonic acid methyl ester.

WORKUP

后处理

  1. temperatureis refluxed for 15 hours
  2. customevaporated
  3. customThe residue is triturated with diethyl ether
  4. filtrationfiltered
  5. customthe filtrate evaporated
  6. customtriturated with the minimum amount of diethyl ether
  7. filtrationthe suspension filtered
  8. customthe filtrate evaporated
  9. distillationthe residue distilled
  10. customthe fraction boiling at 50°-54°/0.1 mm Hg collected