Sodium Hydroxide → 2-Methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid

HRID 1985268ノート

反応式

HRID 1985268 の反応式
C([O:3][C:4](=[O:46])[C:5]([CH3:45])([O:34][C:35]1[CH:40]=[CH:39][C:38]([C:41]([F:44])([F:43])[F:42])=[CH:37][CH:36]=1)[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH2:14][CH2:15][CH:16]2[CH2:20][N:19]([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=3)[C:18](=[O:32])[N:17]2[CH3:33])[CH:8]=1)C.[OH-].[Na+]>C(O)C>[CH3:45][C:5]([O:34][C:35]1[CH:36]=[CH:37][C:38]([C:41]([F:43])([F:42])[F:44])=[CH:39][CH:40]=1)([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH2:14][CH2:15][CH:16]2[CH2:20][N:19]([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:29])([F:30])[F:31])=[CH:24][CH:23]=3)[C:18](=[O:32])[N:17]2[CH3:33])[CH:8]=1)[C:4]([OH:46])=[O:3]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 865962322-Methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid ethyl ester

生成物 1

HCID 865962332-Methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid収率 100%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid ethyl ester (0.113 g, 0.173 mmol) in ethanol (12 mL) was treated with aqueous 5 N NaOH (2 mL) and heated to reflux 1 h. The reaction mixture was cooled, the solvent removed in vacuo. The resultant residue was acidified with aqueous 1 N HCl (15 mL) and extracted with CH2Cl2. The organic layer was dried (Na2SO4) and the solvent removed in vacuo to afford 0.108 g (100%) 2-methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid. 1H NMR. HRMS (ES+) m/z exact mass calc'd for C31H31N2O5F6 (M+1) 625.2137. Found m/z 625.2134.

後処理

  1. temperatureheated
  2. temperatureto reflux 1 h
  3. temperatureThe reaction mixture was cooled
  4. customthe solvent removed in vacuo
  5. extractionextracted with CH2Cl2
  6. dry with materialThe organic layer was dried (Na2SO4)
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-36d70cabbc1440758aeeb2a5f179ef2e
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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