HRID1658244
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 2-hydroxymethyl-5-nitro-N,N-dimethylbenzamide (17 g.) in glacial acetic acid (340 ml.) was added chromium trioxide (17 g.) in water (17 ml.) and glacial acetic acid (340-1). The reaction mixture was stirred at room temperature for 5 minutes, and then poured into ice-water (2 liters). The aqueous was extracted with chloroform (3 × 500 ml.). The chloroform extracts were combined and neutralised by washing with 10% sodium bicarbonate solution. The chloroform exracts were then washed thoroughly with water and dried over magnesium sulphate. The solution was then filtered and the solvent evaporated off to yeild a gum.
WORKUP
后处理
- extractionThe aqueous was extracted with chloroform (3 × 500 ml.)
- washby washing with 10% sodium bicarbonate solution
- washThe chloroform exracts were then washed thoroughly with water
- dry with materialdried over magnesium sulphate
- filtrationThe solution was then filtered
- customthe solvent evaporated off