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Calcium Chloride → 4-[3-(1H-Imidazol-1-yl)propyl]aniline

HRID 856727
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HRID 856727 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][N:13]2[CH:17]=[CH:16][N:15]=[CH:14]2)=[CH:6][CH:5]=1)([O-])=O.[Cl-].[Ca+2].[Cl-]>C(O)C>[N:13]1([CH2:12][CH2:11][CH2:10][C:7]2[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][CH:6]=2)[CH:17]=[CH:16][N:15]=[CH:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5284359Calcium ChlorideHCID 101052881-[3-(4-Nitrophenyl)propyl]imidazole

생성물 1

HCID 214815934-[3-(1H-Imidazol-1-yl)propyl]aniline수율 73.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-[3-(4-nitrophenyl)propyl]imidazole (1.2 g) was dissolved in 85% ethanol solution (37 ml), calcium chloride (0.30 g) and reduced iron (1.5 g) were added to the mixture, and the mixture was heated to reflux for 4 hours. After cooling to room temperature, the mixture was filtered with Celite, and washed with ethyl acetate. The solvent was removed under reduced pressure, and water was added to the obtained residue, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give 4-[3-(imidazol-1-yl)propyl]aniline (0.77 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 hours
  3. filtrationthe mixture was filtered with Celite
  4. washwashed with ethyl acetate
  5. customThe solvent was removed under reduced pressure, and water
  6. additionwas added to the obtained residue
  7. extractionthe mixture was extracted with ethyl acetate
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over magnesium sulfate
  10. customThe solvent was removed under reduced pressure
  11. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a3f6a8451ea44fd6b3978e1f88949799
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262185B2

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