HRID2398047

反应详情

EQUATION

反应方程式

HRID 2398047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 30 g. of γ -valerolactone, 30 ml. of distilled thionyl chloride and 0.5 g. of zinc chloride was heated on a steam bath overnight and then distilled at 15 mm. The distillate was redistilled at 69- 70° and 15 mm. giving 34 g. of 4-chlorovaleryl chloride. The acid chloride was reduced catalytically, reacted with 5-chlorosalicylhydroxamic acid and the resulting intermediate was ring-closed according to the method described in Example 3. The product after recrystallization from trichloroethylene weighed 8.5 g. and melted at 210- 213° C.

WORKUP

后处理

  1. additionA mixture of 30 g
  2. distillationdistilled at 15 mm
  3. distillationThe distillate was redistilled at 69- 70°
  4. customgiving 34 g
  5. customthe resulting intermediate was ring-closed
  6. customThe product after recrystallization from trichloroethylene