반응 #4933

반응 방정식

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

N-methylaniline

→

pale brown crystals

수율 31.0%

2,3-Dihydro-4-methyl-2-[2-(methylphenylamino)ethyl]pyrido[3,2-f][1,4]oxazepin-5(4H)-one

수율 31.0%

반응 조건

후처리

1. 1
   기타Excess N-methylaniline was removed by rotary evaporation (95° C., vacuum pump)
2. 2
   세척washed with dilute aqueous sodium hydroxide (30 ml)
3. 3
   건조dried over sodium sulfate
4. 4
   여과filtered
5. 5
   농축concentrated by rotary evaporation
6. 6
   workup.DISSOLUTIONThe remaining residue was dissolved in ethyl acetate (50 ml)
7. 7
   기타purified by high pressure liquid chromatography
8. 8
   기타After purification, crystals
9. 9
   기타formed from ethyl acetate
10. 10
    기타These crystals were recrystallized from ethyl acetate

실험 절차

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one hydrochloride, 4.00 g (0.015 mole) was dissolved in N-methylaniline (30 ml) and heated to 95° C. with stirring for 2 days. Excess N-methylaniline was removed by rotary evaporation (95° C., vacuum pump). The residue was taken up in chloroform (80 ml) and washed with dilute aqueous sodium hydroxide (30 ml). The chloroform layer was decolorized with activated carbon and dried over sodium sulfate, filtered and concentrated by rotary evaporation. The remaining residue was dissolved in ethyl acetate (50 ml) and purified by high pressure liquid chromatography using a silica gel column and ethyl acetate as the eluent. After purification, crystals formed from ethyl acetate. These crystals were recrystallized from ethyl acetate, giving 1.40 g (31%) of pale brown crystals.

출처