反应详情

To a solution of 16.6 g (0.06 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one in 150 ml of dry toluene was added a mixture of 8.6 g (0.045 mole) of phosphorus pentasulfide and 8.6 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. Yellow solid, 6.5 g (35%) was obtained which was recrystallized from ethanol, m.p. 166°-168° C.

1. temperatureheated
2. temperatureat reflux for 24 hr
3. filtrationThe mixture was filtered hot
4. concentrationthe filtrate concentrated under reduced pressure
5. customYellow solid, 6.5 g (35%) was obtained which
6. customwas recrystallized from ethanol, m.p. 166°-168° C.