HRID2186453

反应详情

EQUATION

反应方程式

HRID 2186453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-methyl-3-trifluoromethylisoxazole-4-carboxylic acid ethyl ester (2.0 g) and sodium hydroxide (1.1 g) in tetrahydrofuran/water (20 ml/20 ml) was heated at reflux for 18 hours. The tetrahydrofuran was removed in vacuo and the aqueous residue washed with ethyl acetate (50 ml), acidified to pH2 with conc. hydrochloric acid and extracted with ethyl acetate (100 ml). The organic layer was washed with brine (50 ml), separated, dried over magnesium sulphate, filtered and concentrated in vacuo to afford the title compound as a peach-coloured solid (1.4 g).

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. customThe tetrahydrofuran was removed in vacuo
  3. washthe aqueous residue washed with ethyl acetate (50 ml)
  4. extractionextracted with ethyl acetate (100 ml)
  5. washThe organic layer was washed with brine (50 ml)
  6. customseparated
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo