反应详情

A mixture of 1.74 g (5.14 mmol) of (±) trans-(5,6,6a,7,8,9,10,10a-octahydropyrido[2,3-h]quinazolin-2-yl)-carbamic acid, phenylmethyl ester, (Example 20), 3.6 g (26.05 mmol) of finely ground potassium carbonate and 2.5 ml (25.63 mmol) of 1-iodopropane in 250 ml acetonitrile is refluxed, under nitrogen, for 24 hours. The suspension is cooled, filtered through a pad of Celite, concentrated and partitioned between brine and chloroform. The chloroform extract is separated, dried over magnesium sulfate, filtered and concentrated to a viscous brown oil. Medium pressure chromatography (silica gel, 2% ammonium hydroxide-98% ethyl acetate) afforded 1.41 g (72%) of the title compound as a white solid; mp 174°-177° C.

1. temperatureis refluxed, under nitrogen, for 24 hours
2. temperatureThe suspension is cooled
3. filtrationfiltered through a pad of Celite
4. concentrationconcentrated
5. custompartitioned between brine and chloroform
6. extractionThe chloroform extract
7. customis separated
8. dry with materialdried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated to a viscous brown oil