HRID582486

反应详情

EQUATION

反应方程式

HRID 582486 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.48 g (14.9 mmol) rac-2,4-Dibromo-N-isobutyl-butyramide were dissolved in 40 ml dichloromethane, then 17.3 ml of 50% sodium hydroxide solution and 0.48 g Dowex 2×10 were added. The mixture was stirred vigorously for 4 h at room temperature. Afterwards the mixture was poured into 50 ml ice/water an the phases were separated. The aqueous phase was extracted thrice with 20 ml dichloromethane, and the combined organic phases were washed once with 20 ml water, once with 20 ml brine and dried over magnesium sulfate. After evaporation of the solvent, the resulting colourless oil was chromatographed or silica gel (0.040-0.063 mm) with ethyl acetate/n-hexane 1:1 as eluent.

WORKUP

后处理

  1. customwere separated
  2. extractionThe aqueous phase was extracted thrice with 20 ml dichloromethane
  3. washthe combined organic phases were washed once with 20 ml water, once with 20 ml brine
  4. dry with materialdried over magnesium sulfate
  5. customAfter evaporation of the solvent
  6. customthe resulting colourless oil was chromatographed