HRID278407

反应详情

EQUATION

反应方程式

HRID 278407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

9.70 g of 5-hydroxy-3-methyl-4-(3-methylisooxazol-5-yl)isoxazole was added to 18 ml of acetic acid and 30 ml of methanol, and was heated to 60° C. to dissolve. To the resulting solution was added 3.20 g of electrolytic iron powder to stir for an hour at 60° C. 20 ml of 3N hydrochloric acid was further added to the reaction solution to stir for 20 minutes at 60° C. The reaction mixture was cooled to room temperature and water was added. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated salt water, dried over anhydrous magnesium sulfate and concentrated to give 6.00 g of the title compound as a reddish brown liquid.

WORKUP

后处理

  1. dissolutionto dissolve
  2. stirringto stir for 20 minutes at 60° C
  3. temperatureThe reaction mixture was cooled to room temperature
  4. extractionThe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated salt water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated