HRID2186453
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 18 hours
- customThe tetrahydrofuran was removed in vacuo
- washthe aqueous residue washed with ethyl acetate (50 ml)
- extractionextracted with ethyl acetate (100 ml)
- washThe organic layer was washed with brine (50 ml)
- customseparated
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- concentrationconcentrated in vacuo