2-(4-{2-[1-(3,4-Dimethyl-benzyl)-3-(4-methoxy-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester → 2-(4-{2-[1-(3,4-Dimethyl-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester

HRID 1985236

反応式

HRID 1985236 の反応式
[CH2:1]([O:3][C:4](=[O:42])[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH:18]2[CH2:22][N:21]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[C:26]([CH3:31])[CH:25]=3)[C:20](=[O:32])[N:19]2CC2C=CC(OC)=CC=2)=[CH:11][CH:10]=1)([CH3:7])[CH3:6])[CH3:2]>FC(F)(F)C(O)=O.O>[CH2:1]([O:3][C:4](=[O:42])[C:5]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:16][CH2:17][CH:18]2[CH2:22][N:21]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[C:26]([CH3:31])[CH:25]=3)[C:20](=[O:32])[NH:19]2)=[CH:13][CH:14]=1)([CH3:6])[CH3:7])[CH3:2]

参加物

4

反応物 1

HCID 577189882-(4-{2-[1-(3,4-Dimethyl-benzyl)-3-(4-methoxy-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester

生成物 1

HCID 577193032-(4-{2-[1-(3,4-Dimethyl-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester収率 60.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 2-(4-{2-[1-(3,4-dimethyl-benzyl)-3-(4-methoxy-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester (2.51 g, 4.36 mmol) in trifluoroacetic acid (70 mL) was stirred at room temperature under N2 for 1 h. The reaction was diluted with water, and extracted with Et2O. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using 98:2 CH2Cl2:MeOH to afford 1.20 g (60%) 2-(4-{2-[1-(3,4-dimethyl-benzyl)-2-oxo-imidazolidin-4-yl]-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester. MS (ES+) Calc'd for C26H35N2O5 (M+1) 455. Found m/z 455 (100%). 1H NMR.

後処理

  1. extractionextracted with Et2O
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customto afford crude product that
  5. customwas purified by flash chromatography

出典と根拠

ORDレコード
ord-38ef302e11254772a8d7233cc191f0d4
出典データセット
uspto-grants-2009_06
特許番号
US07544812B2

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