반응 #4946

반응 방정식

dimethylamine

sodium iodide

2-(2-chloropropyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one

→

2-[2-(Dimethylamino)propyl]-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one dihydrochloride

반응 조건

후처리

1. 1
   기타The bomb was sealed tightly
2. 2
   기타placed in the oven at 60° C.
3. 3
   workup.WAITto stand at room temperature for several days
4. 4
   기타separated via column chromatography
5. 5
   세척eluting with ethanol
6. 6
   workup.ADDITIONThe fractions containing the desired product
7. 7
   농축concentrated by rotary evaporation (80° C., 30 mm)
8. 8
   세척washed with 2×50 ml diluted sodium hydroxide
9. 9
   기타The chloroform was removed by rotary evaporation (70° C., 30 mm)
10. 10
    workup.ADDITIONthe residue treated with ethereal hydrogen chloride and hydrogen chloride in isopropyl alcohol
11. 11
    기타The white crystals which were collected

실험 절차

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.

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