HRID1762498
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
1400 g of a crude N-methoxy-2,4-dibromobutanamide was dissolved in 5 liters of benzene. Then 125 g of NaH was added little by little to the solution at 15° to 20° C. while the reaction mixture was cooled with an iced water bath. After the reaction, the remaining NaH was decomposed with ice and the product mixture was washed with a saturated, aqueous salt solution. It was dried with magnesium sulfate. Then benzene was distilled out. The product was purified with the column chromatography, using silica gel and a mixture of acetaone and benzene to obtain 500 g of the title compound 4.
WORKUP
后处理
- temperaturewas cooled with an iced water bath
- customAfter the reaction
- washthe product mixture was washed with a saturated, aqueous salt solution
- dry with materialIt was dried with magnesium sulfate
- distillationThen benzene was distilled out
- customThe product was purified with the column chromatography
- additiona mixture of acetaone and benzene