HRID1984643
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
3-(5-Methyl-3-phenyl-isoxazol-4-ylethynyl)-benzoic acid methyl ester (600 mg, 1.89 mmol) was treated with ethanol (12 mL) and aqueous sodium hydroxide (1 M, 7.56 mL, 7.56 mmol). The reaction mixture was heated for 1.5 h at 80° C. After concentration and dilution with water (9 mL) the pH was adjusted to 1.5 by adding hydrochloric acid (1 M, 8 mL). The resulting suspension was stirred for 30 min at 0° C. and filtered. Washing with ice-cold water (10 mL) and drying afforded the title compound (546 mg, 95%) as a light brown solid. MS: m/e=304.1 [M+H]+.
WORKUP
后处理
- concentrationAfter concentration and dilution with water (9 mL) the pH
- additionby adding hydrochloric acid (1 M, 8 mL)
- filtrationfiltered
- washWashing with ice-cold water (10 mL)
- customdrying