HRID1762498

反应详情

EQUATION

反应方程式

HRID 1762498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas cooled with an iced water bath
  2. customAfter the reaction
  3. washthe product mixture was washed with a saturated, aqueous salt solution
  4. dry with materialIt was dried with magnesium sulfate
  5. distillationThen benzene was distilled out
  6. customThe product was purified with the column chromatography
  7. additiona mixture of acetaone and benzene