反应详情

To a solution of 59 g (0.25 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride in 1500 ml of chloroform was added 41.5 g (0.19 mole) of phosphorus pentasulfide and the mixture was heated to reflux for 18 hr. The mixture was filtered and the filtrate was extracted with dilute sodium hydroxide. The chloroform layer was concentrated and the residue was dissolved in 250 ml of boiling isopropyl alcohol. On cooling, 28 g (44%) of yellow solid precipitated. A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

1. temperaturethe mixture was heated
2. temperatureto reflux for 18 hr
3. filtrationThe mixture was filtered
4. extractionthe filtrate was extracted with dilute sodium hydroxide
5. concentrationThe chloroform layer was concentrated
6. dissolutionthe residue was dissolved in 250 ml of boiling isopropyl alcohol
7. temperatureOn cooling
8. custom28 g (44%) of yellow solid precipitated
9. customA portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.