反应详情

A 2 liter round-bottom flask equipped with a magnetic stirring bar and reflux condenser with a nitrogen inlet was charged with 115.0 g (0.506 mole) of dibenzo[b,f][1,4]thiazepine-11(10-H)one, phosphorous oxychloride 700 ml (7.5 moles) and N,N-dimethylaniline 38.0 g (0.313 mole). The grey suspension was heated to gentle refluxing using a heating mantle. After 6 hours of heating, the resulting amber solution was allowed to cool to room temperature (from about 18°-25°C.) and was analyzed by thin-layer chromatography (TLC) using silica gel plates, developed with ether-hexane (1:1) and detected with ultraviolet light. Analysis revealed the desired imino chloride, Rf =0.70, and an absence of starting lactam.

1. customA 2 liter round-bottom flask equipped with a magnetic stirring bar
2. temperaturereflux condenser with a nitrogen inlet
3. temperatureThe grey suspension was heated
4. temperatureto gentle refluxing
5. temperatureAfter 6 hours of heating