反应详情

To 70 ml of freshly collected dimethylamine was added 5.0 g (0.017 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4,8-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one and 5 ml of methanol. The reaction flask was sealed tightly and left standing at room temperature for 2 days. The reaction flask was cooled and opened and the solvent evaporated in a stream of air. The residue was taken up in 100 ml of methylene chloride and the solution was washed with 3×50 ml of 1N sodium hydroxide, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residual oil was treated with 2 equivalents of fumaric acid in isopropyl alcohol which yielded 5.3 g (59%) of white analytically pure crystals, m.p. 153°-56° C.

1. customThe reaction flask was sealed tightly
2. waitleft
3. temperatureThe reaction flask was cooled
4. customthe solvent evaporated in a stream of air
5. washthe solution was washed with 3×50 ml of 1N sodium hydroxide
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation
9. customyielded 5.3 g (59%) of white analytically pure crystals, m.p. 153°-56° C.