反应详情

Into a stainless steel bomb was placed 1.0 g sodium iodide, 5.0 g (0.017 mole) of 2-(2-chloropropyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one and 40 ml of dimethylamine. The bomb was sealed tightly, placed in the oven at 60° C. and rolled continuously for 7 days. The bomb was allowed to stand at room temperature for several days. The residue was combined with that of a previous run of equal size and separated via column chromatography using silica gel and eluting with ethanol and then with 3% triethylamine/ethanol. The fractions containing the desired product were combined and concentrated by rotary evaporation (80° C., 30 mm). The residue was taken up in 150 ml of chloroform and washed with 2×50 ml diluted sodium hydroxide. The chloroform was removed by rotary evaporation (70° C., 30 mm) and the residue treated with ethereal hydrogen chloride and hydrogen chloride in isopropyl alcohol. The white crystals which were collected weighed 3 g (28%), m.p. 173°-76° C.

1. customThe bomb was sealed tightly
2. customplaced in the oven at 60° C.
3. waitto stand at room temperature for several days
4. customseparated via column chromatography
5. washeluting with ethanol
6. additionThe fractions containing the desired product
7. concentrationconcentrated by rotary evaporation (80° C., 30 mm)
8. washwashed with 2×50 ml diluted sodium hydroxide
9. customThe chloroform was removed by rotary evaporation (70° C., 30 mm)
10. additionthe residue treated with ethereal hydrogen chloride and hydrogen chloride in isopropyl alcohol
11. customThe white crystals which were collected