HRID273665

反应详情

EQUATION

反应方程式

HRID 273665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(2-benzoylethyl)-N,N,N-trimethylammonium iodide (5.0 g) was suspended in water (400 ml) and the mixture passed through the CMR (15 ml/min; 90°-95° C.; atmospheric pressure) and the hot product collected in a mixture of ice (250 g) and diethyl ether (100 ml), in a flask which was cooled in an ice bath. The ether phase was separated and the aqueous extracted with ether (3×150 ml). The pooled organic phase was dried over anhydrous sodium sulphate and evaporated to dryness, affording phenylvinyl ketone as a colourless oil (1.95 g; 94% yield) in high purity, according to the 1H NMR spectrum; cf ref.15, where a yield of 51% was obtained.

WORKUP

后处理

  1. custompassed through the CMR (15 ml/min; 90°-95° C.; atmospheric pressure)
  2. customthe hot product collected in a mixture of ice (250 g) and diethyl ether (100 ml), in a flask which
  3. temperaturewas cooled in an ice bath
  4. customThe ether phase was separated
  5. extractionthe aqueous extracted with ether (3×150 ml)
  6. dry with materialThe pooled organic phase was dried over anhydrous sodium sulphate
  7. customevaporated to dryness