HRID1482863

反应详情

EQUATION

反应方程式

HRID 1482863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-bromo-N,2-dihydroxybenzamide (4.12 g, 17.76 mmol) was suspended in 100 mL THF. Carbonyldiimidazole (5.76 g, 35.5 mmol) was added and the mixture was heated under reflux for three hours. The solvent was evaporated under vacuum, 100 mL water was added and the solution was acidified to pH 1 with 1N HCl under rapid stirring. The formed precipitate was filtered, washed with water and dried, giving 5-bromobenzo[d]isoxazol-3-ol (3.71 g, 17.3 mmol) as off-white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for three hours
  3. customThe solvent was evaporated under vacuum, 100 mL water
  4. additionwas added
  5. filtrationThe formed precipitate was filtered
  6. washwashed with water
  7. customdried