HRID1984643

反应详情

EQUATION

反应方程式

HRID 1984643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationAfter concentration and dilution with water (9 mL) the pH
  2. additionby adding hydrochloric acid (1 M, 8 mL)
  3. filtrationfiltered
  4. washWashing with ice-cold water (10 mL)
  5. customdrying