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HCID 20131146, 화합물 → 1-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole

HRID 1285378
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HRID 1285378 반응식
[N:1]([CH:4]([CH2:11][O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[CH2:5][N:6]1[CH:10]=[CH:9][N:8]=[CH:7]1)=[N+]=[N-].[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[NH2:1][CH:4]([CH2:11][O:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=1)[CH2:5][N:6]1[CH:10]=[CH:9][N:8]=[CH:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 20131146HCID 20131146, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 201311651-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole수율 77.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 1-[2-azido-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole (5.1 g, 0.018M) in dry tetrahydrofuran (10 ml) was added dropwise to a stirred slurry of lithium aluminium hydride (0.68 g, 0.018M) in dry tetrahydrofuran (40 ml) at room temperature under a stream of dry nitrogen. When the addition was complete the reaction mixture was heated under reflux for 18 hours. The solvent was evaporated off under reduced pressure and the residue was extracted with ethyl acetate, washed with saturated aqueous ammonium chloride solution and dried (MgSO4). The solvent was evaporated off under reduced pressure to give 1-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole as an oil (3.6 g) which was used directly without further purification.

후처리

  1. additionWhen the addition
  2. temperaturewas heated
  3. temperatureunder reflux for 18 hours
  4. customThe solvent was evaporated off under reduced pressure
  5. extractionthe residue was extracted with ethyl acetate
  6. washwashed with saturated aqueous ammonium chloride solution
  7. dry with materialdried (MgSO4)
  8. customThe solvent was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-b54f1dc69bc243d6a71cd29dc450acca
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04567189

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