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Ethanol → Methyl 3-[6-(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl-5-fluoropyridin-3-yl]propionate

HRID 2080433
ノート
印刷プレビュー

反応式

HRID 2080433 の反応式
C(O)C.[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([C:14]2[N:19]=[C:18]([CH2:20][C:21]3[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=3[F:28])[C:17]([CH:29]=[CH:30][C:31]([O:33][CH3:34])=[O:32])=[CH:16][C:15]=2[F:35])(=[O:13])=[O:12])=[CH:7][CH:6]=1>ClCCl>[Cl:4][C:5]1[CH:6]=[CH:7][C:8]([S:11]([C:14]2[N:19]=[C:18]([CH2:20][C:21]3[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=3[F:28])[C:17]([CH2:29][CH2:30][C:31]([O:33][CH3:34])=[O:32])=[CH:16][C:15]=2[F:35])(=[O:12])=[O:13])=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 702EthanolHCID 67101326HCID 67101326、化合物

生成物 1

HCID 23114759Methyl 3-[6-(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl-5-fluoropyridin-3-yl]propionate収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A Raney nickel suspension (“R-100”, product of Nikko Rica Corporation) (1 ml) was washed sequentially with water and ethanol to give an ethanol (10 ml) suspension. The resulting suspension was added to an ethanol (40 ml) solution of methyl 3-[6-(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl-5-fluoropyridin-3-yl]acrylate (1.38 g, 2.86 mmol). Under a hydrogen atmosphere, the resulting mixture was stirred at room temperature for 1 hour. The reaction mixture was filtered through Celite and the filtrate was concentrated under reduced pressure. The residue thus obtained was dissolved in dichloromethane. The resulting solution was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to give the title compound 1.37 g, 2.83 mmol, 99%) as a white solid.

後処理

  1. washA Raney nickel suspension (“R-100”, product of Nikko Rica Corporation) (1 ml) was washed sequentially with water and ethanol
  2. customto give an ethanol (10 ml) suspension
  3. filtrationThe reaction mixture was filtered through Celite
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue thus obtained
  6. dry with materialThe resulting solution was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-9acd0113027c4f55a8ba8e11a538fa16
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932271B2

反応ノート

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