HRID2244625
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 1,3-benzothiazole-6-carboxamide (1.96 g) in POCl3 (10 ml) was refluxed for 4 hours. The reaction solution was concentrated, and water was slowly added thereto at 0° C. It was extracted with EtOAc, and the organic layer was dried over anhydrous MgSO4, and then filtered, and the filtrate was concentrated. The residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 60:40) to obtain 1,3-benzothiazole-6-carbonitrile as a pale yellow solid.
WORKUP
后处理
- concentrationThe reaction solution was concentrated
- additionwater was slowly added
- customat 0° C
- extractionIt was extracted with EtOAc
- dry with materialthe organic layer was dried over anhydrous MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 60:40)