HRID273665
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
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
- custompassed through the CMR (15 ml/min; 90°-95° C.; atmospheric pressure)
- customthe hot product collected in a mixture of ice (250 g) and diethyl ether (100 ml), in a flask which
- temperaturewas cooled in an ice bath
- customThe ether phase was separated
- extractionthe aqueous extracted with ether (3×150 ml)
- dry with materialThe pooled organic phase was dried over anhydrous sodium sulphate
- customevaporated to dryness