Triethylamine → ethyl 5-[[2-(1H-imidazol-1-yl)-1-[[(4-methoxyphenyl)methoxy]methyl]ethyl]amino]-5-oxopentanoate

HRID 1380124ノート

反応式

HRID 1380124 の反応式
Cl[C:2]([CH2:4][CH2:5][CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:3].[NH2:12][CH:13]([CH2:20][O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1)[CH2:14][N:15]1[CH:19]=[CH:18][N:17]=[CH:16]1.C(N(CC)CC)C>ClCCl>[N:15]1([CH2:14][CH:13]([NH:12][C:2](=[O:3])[CH2:4][CH2:5][CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:20][O:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=2)[CH:19]=[CH:18][N:17]=[CH:16]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 78881Ethyl 5-chloro-5-oxovalerateHCID 201311651-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole

生成物 1

HCID 20131172ethyl 5-[[2-(1H-imidazol-1-yl)-1-[[(4-methoxyphenyl)methoxy]methyl]ethyl]amino]-5-oxopentanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of ethyl 4-(chloroformyl)butyrate (0.714 g, 0.004 mol) in dichloromethane (5 ml) was added dropwise to a stirred solution of 1-[2-amino-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole (Example 32c; 1.0 g, 0.0038 mol) and triethylamine (0.4 g, 0.004 mol) in dichloromethane (20 ml) at room temperature. The solution was stirred for 12 hours, washed with an aqueous saturated solution of ammonium chloride and dried (Na2SO4). The solvent was evaporated off under reduced pressure and the crude product was purified by column chromatography (silica gel, 2% ethanol in chloroform) to give ethyl 5-[[2-(1H-imidazol-1-yl)-1-[[(4-methoxyphenyl)methoxy]methyl]ethyl]amino]-5-oxopentanoate as a pale-yellow oil.

後処理

  1. washwashed with an aqueous saturated solution of ammonium chloride
  2. dry with materialdried (Na2SO4)
  3. customThe solvent was evaporated off under reduced pressure
  4. customthe crude product was purified by column chromatography (silica gel, 2% ethanol in chloroform)

出典と根拠

ORDレコード
ord-8c3f9233a06f4700877ba2e0837bd668
出典データセット
uspto-grants-1986_04
特許番号
US04579862

反応ノート

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