반응 #364022

반응 방정식

morpholine

3-bromopropanol

→

title compound

3-Morpholinopropanol

용매

toluene

반응 조건

후처리

1. 1
   기타The cooling bath was then removed
2. 2
   온도The mixture was heated at 100° C. (bath temperature) for 3 hrs under argon
3. 3
   온도After cooling
4. 4
   workup.ADDITIONthe mixture was diluted with ethyl acetate
5. 5
   세척The organic layer was washed (brine)
6. 6
   건조dried (MgSO4)
7. 7
   농축concentrated
8. 8
   기타The residue was chromatographed
9. 9
   세척(silica gel, elution by 1:1 CH2Cl2-hexane)

실험 절차

To a cooled (0° C., ice bath) solution of morpholine (31.5 ml, 0.36 mole) in toluene (300 ml) was added 3-bromopropanol (25 g, 0.18 mole) under argon. The cooling bath was then removed, the resulting mixture was warmed to room temperature, and stirred at room temperature for 1 hr. The mixture was heated at 100° C. (bath temperature) for 3 hrs under argon. After cooling, the mixture was diluted with ethyl acetate. The organic layer was washed (brine), dried (MgSO4), and concentrated. The residue was chromatographed (silica gel, elution by 1:1 CH2Cl2-hexane) to give the title compound as a clear oil.

출처