HRID1696917
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 2,6-dichloro-4-methyl-nicotinamide (6.40 g) in 2:1 acetic anhydride/acetic acid (156 mL) was treated with sodium nitrite (21.5 g), stirred for 18 hours, poured into diethyl ether (600 mL) and filtered. The filtrate was concentrated with a toluene azeotrope, and the concentrate was treated with brine and extracted with ethyl acetate. The extract was dried (MgSO4), filtered, and concentrated; and this concentrate was suspended in hexane, sonicated and filtered.
WORKUP
后处理
- filtrationfiltered
- concentrationThe filtrate was concentrated with a toluene azeotrope
- additionthe concentrate was treated with brine
- extractionextracted with ethyl acetate
- dry with materialThe extract was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customsonicated
- filtrationfiltered