HRID278404

反应详情

EQUATION

反应方程式

HRID 278404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g of 3-methylisooxazol-5-yl-2,4,8-nonanetrione obtained in Example 6 was dissolved in 15 ml of ethanol, and 0.53 g of triethylamine was added to it to stir at reflux for 8 hours. After cooling, the reaction solution was poured into ice water, acidified with hydrochloric acid and extracted with ethyl acetate. The ethyl-acetate layer was washed with water, dehydrated over anhydrous magnesium sulfate, and concentrated. The obtained residue was purified on silica gel column chromatography to give 0.36 g of the title compound as white crystals. Melting point: 104-105° C.

WORKUP

后处理

  1. temperatureat reflux for 8 hours
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe ethyl-acetate layer was washed with water
  5. concentrationconcentrated
  6. customThe obtained residue was purified on silica gel column chromatography