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Acetonitrile → Ethyl[5-(3,5-difluorophenyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate

HRID 1685380
ノート
印刷プレビュー

反応式

HRID 1685380 の反応式
C([CH:3]([N:7]1[C:11]([C:13]2[CH:18]=[C:17]([F:19])[CH:16]=[C:15]([F:20])[CH:14]=2)([CH3:12])[C:10](=[O:21])[N:9](CC2C=CC(OC)=CC=2)[C:8]1=[O:31])[C:4]([O-:6])=[O:5])C.[N+]([O-])([O-])=O.[Ce+4].[NH4+].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[CH3:54][C:55]#N>O>[CH2:54]([O:6][C:4](=[O:5])[CH2:3][N:7]1[C:11]([C:13]2[CH:18]=[C:17]([F:19])[CH:16]=[C:15]([F:20])[CH:14]=2)([CH3:12])[C:10](=[O:21])[NH:9][C:8]1=[O:31])[CH3:55]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 9869224Ammonium cerium (IV) nitrateHCID 131729539(+/-)-Ethyl[5-(3,5-difluorophenyl)-3-(4-methoxybenzyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate

生成物 1

HCID 91574597Ethyl[5-(3,5-difluorophenyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a stirred solution of (±)-ethyl[5-(3,5-difluorophenyl)-3-(4-methoxybenzyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate from Step C (11.4 g, 26.3 mmol) in CH3CN (150 mL) was added drop wise a solution of ammonium cerium (IV) nitrate (43.2 g, 78.8 mmol) in water (100 mL) and the resulting mixture was stirred at ambient temperature for 3 h. The reaction was diluted with water (300 mL) and extracted with EtOAc (3×250 mL). The combined organic extracts were washed with water (50 mL), saturated NaHCO3 (50 mL), and brine (50 mL), dried over MgSO4, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of hexane:EtOAc—100:0 to 50:50, to give the racemic title compound. The enantiomers were resolved by HPLC, utilizing a ChiralPak AD column and eluting with hexane:EtOH:DEA 40:60:1. The first major peak to elute was ethyl[5-(3,5-difluorophenyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate, isomer A, the title compound, and the second major peak to elute was ethyl[5-(3,5-difluorophenyl)-5-methyl-2,4-dioxoimidazolidin-1-yl]acetate, isomer B. MS: m/z=313 (M+1).

後処理

  1. extractionextracted with EtOAc (3×250 mL)
  2. washThe combined organic extracts were washed with water (50 mL), saturated NaHCO3 (50 mL), and brine (50 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified by silica gel chromatography
  7. washeluting with a gradient of hexane

出典と根拠

ORDレコード
ord-1dd04a8e5bd0421f86fbf350a246928e
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148390B2

反応ノート

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