HRID1981222

反应详情

EQUATION

反应方程式

HRID 1981222 的结构方程式

PROCEDURE

实验过程

Methyl formylbutyrate (13 g) and 1-triphenylphosphoranylidene-2-propanone (31.4 g) were refluxed together in toluene (200 ml) for 30 minutes. The toluene was then evaporated off and ether (200 ml) added to the residue to give a suspension which was stirred at room temperature for 5 minutes. The suspended triphenylphosphine oxide was filtered off and washed with a further 100 ml of ether. The combined ether solutions were evaporated to dryness to give a yellow oil which was distilled at 0.1 mm Hg using a Kugelrohr apparatus (air bath temperature 140° C.) to yield 7-oxo-5-octenoic acid methyl ester as a colourless oil.

WORKUP

后处理

  1. customThe toluene was then evaporated off
  2. additionether (200 ml) added to the residue
  3. customto give a suspension which
  4. filtrationThe suspended triphenylphosphine oxide was filtered off
  5. washwashed with a further 100 ml of ether
  6. customThe combined ether solutions were evaporated to dryness
  7. customto give a yellow oil which
  8. distillationwas distilled at 0.1 mm Hg
  9. customa Kugelrohr apparatus (air bath temperature 140° C.)