HRID329780

反应详情

EQUATION

反应方程式

HRID 329780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thionyl chloride (118 g) was added to 5-methylisoxazol-4-yl carboxylic acid (42 g) and stirred at room temperature as dimethylformamide (0.2 ml) was added. The solution was heated under reflux for 2 hours with stirring. Excess thionyl chloride was removed in vacuo at 50° C., then the residue was distilled through a 15 cm Vigreaux column at reduced pressure to give an oil, b.p. 32°-34° C./0.1 mm Hg.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe solution was heated
  3. temperatureunder reflux for 2 hours
  4. customExcess thionyl chloride was removed in vacuo at 50° C.
  5. distillationthe residue was distilled through a 15 cm Vigreaux column at reduced pressure
  6. customto give an oil, b.p. 32°-34° C./0.1 mm Hg