HRID1038397
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
To a solution of 4.0 g (27.4 mmol) 1H-indazole-5-carbaldehyde [preparation described in US 2005/0227968-A1 (Intermediate 1)] in acetonitrile (116 ml) were added 4.2 g (31.5 mmol) N-chlorosuccinimide at room temperature. The resulting solution was stirred under reflux for 12 h. The mixture was then concentrated under reduced pressure yielding a solid precipitate. This material was triturated with water, filtered, and dried under high vacuum for 12 h to give the title compound (4.8 g, 97% of th.) as a white solid.
WORKUP
后处理
- temperatureunder reflux for 12 h
- concentrationThe mixture was then concentrated under reduced pressure
- customyielding a solid precipitate
- customThis material was triturated with water
- filtrationfiltered
- customdried under high vacuum for 12 h