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Triethylamine → HCID 20222380, 화합물

HRID 980222
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HRID 980222 반응식
[NH2:1][CH:2]([CH2:9][O:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1)[CH2:3][N:4]1[CH:8]=[CH:7][N:6]=[CH:5]1.C(N(CC)CC)C.[CH3:27][O:28][C:29]1[CH:36]=[CH:35][C:32]([CH2:33]Cl)=[CH:31][CH:30]=1>C(#N)C>[CH3:27][O:28][C:29]1[CH:36]=[CH:35][C:32]([CH2:33][NH:1][CH:2]([CH2:9][O:10][CH2:11][C:12]2[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=2)[CH2:3][N:4]2[CH:8]=[CH:7][N:6]=[CH:5]2)=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 699934-Methyloxybenzyl chlorideHCID 201311651-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole

생성물 1

HCID 20222380HCID 20222380, 화합물수율 3.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 1-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole (1.70 g, 0.0065M) in dry acetonitrile (10 ml) containing triethylamine (0.5 ml) was treated with 4-methoxybenzyl chloride (1.12 g, 0.0072M) and heated under reflux for 18 hours under a stream of dry nitrogen. The solvent was evaporated off under reduced pressure and the residue was extracted with ethyl acetate, washed with saturated aqueous sodium hydrogen carbonate solution and dried (MgSO4). The solvent was evaporated off under reduced pressure to give the crude product as an oil which was further purified by chromatography (silica gel), 10% ethanol in chloroform) to give N-[(4-methoxyphenyl)methyl]-α-[[(4-methoxyphenyl)methoxy]methyl]-1H-imidazole-1-ethanamine (0.09 g ) as a pale yellow oil.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 18 hours under a stream of dry nitrogen
  3. customThe solvent was evaporated off under reduced pressure
  4. extractionthe residue was extracted with ethyl acetate
  5. washwashed with saturated aqueous sodium hydrogen carbonate solution
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated off under reduced pressure
  8. customto give the crude product as an oil which
  9. customwas further purified by chromatography (silica gel), 10% ethanol in chloroform)

출처 및 근거

ORD 기록
ord-770916f59a084b4f882ba95772c44e01
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04636518

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