Sodium hydride → 2-Butoxy-2-methyl-3-(4-{2-[3-methyl-2-oxo-1-(3-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-propionic acid ethyl ester

HRID 1985156ノート

反応式

HRID 1985156 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6]Br.[CH2:13]([O:15][C:16](=[O:41])[C:17]([O:36][CH2:37][CH2:38][CH2:39][CH3:40])([CH3:35])[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH:28]2[CH2:32][NH:31][C:30](=[O:33])[N:29]2[CH3:34])=[CH:21][CH:20]=1)[CH3:14].[H-].[Na+]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH2:13]([O:15][C:16](=[O:41])[C:17]([O:36][CH2:37][CH2:38][CH2:39][CH3:40])([CH3:35])[CH2:18][C:19]1[CH:20]=[CH:21][C:22]([O:25][CH2:26][CH2:27][CH:28]2[CH2:32][N:31]([CH2:6][C:5]3[CH:8]=[CH:9][CH:10]=[C:3]([C:2]([F:12])([F:11])[F:1])[CH:4]=3)[C:30](=[O:33])[N:29]2[CH3:34])=[CH:23][CH:24]=1)[CH3:14]

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 1230611-(Bromomethyl)-3-(trifluoromethyl)benzeneHCID 688675082-Butoxy-2-methyl-3-{4-[2-(3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-propionic acid ethyl ester

生成物 1

HCID 688684932-Butoxy-2-methyl-3-(4-{2-[3-methyl-2-oxo-1-(3-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-propionic acid ethyl ester

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 8857Ethyl Acetate溶媒

実験手順

3-Trifluoromethylbenzyl bromide (0.037 g, 0.157 mmol) and tetrabutyl ammonium iodide (catalytic amount) are added to a 0° C. suspension of 2-Butoxy-2-methyl-3-{4-[2-(3-methyl-2-oxo-imidazolidin-4-yl)-ethoxy]-phenyl}-propionic acid ethyl ester (0.043 g, 0.105 mmol) and sodium hydride (0.010 g, 0.26 mmol, 60% suspension on mineral oil), pre-stirred for 1 h at ambient temperature. The reaction mixture is stirred at ambient temperature for 48 h, diluted with ethyl acetate, and washed with 1N HCl and water. The organic layer is dried over MgSO4, concentrated in vacuo, and used in the next step. MS [EI+] 565 (M+H)+.

後処理

  1. stirringThe reaction mixture is stirred at ambient temperature for 48 h
  2. washwashed with 1N HCl and water
  3. dry with materialThe organic layer is dried over MgSO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4fd251ca823a4387829cc10ca27c785c
出典データセット
uspto-grants-2009_06
特許番号
US07544812B2

反応ノート

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