反应详情

To a solution of 3.5 g (0.0145 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepine-5(4H)-one in ethanol (15 ml) was added 2-methyl pyrrolidine (5.0 g, 0.063 mole). The solution was heated to reflux for 3 hours with stirring. The ethanol was removed by rotary evaporation (water aspirator, 80° C.). The residual oil was partitioned between dilute aqueous sodium hydroxide (50 ml) and chloroform (50 ml). The organic layer was saved and the aqueous layer extracted with chloroform (2×30 ml). All the chloroform layers were combined, dried over anhydrous sodium sulfate and concentrated by rotary evaporation (water aspirator, 70° C.). The residual oil was then distilled at 200° C. and low vacuum (vacuum pump) giving 1.5 g (36.7%) of a clear oil.

1. temperatureThe solution was heated
2. temperatureto reflux for 3 hours
3. customThe ethanol was removed by rotary evaporation (water aspirator, 80° C.)
4. customThe residual oil was partitioned between dilute aqueous sodium hydroxide (50 ml) and chloroform (50 ml)
5. extractionthe aqueous layer extracted with chloroform (2×30 ml)
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated by rotary evaporation (water aspirator, 70° C.)
8. distillationThe residual oil was then distilled at 200° C.