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

HRID 2080433
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HRID 2080433 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 702EthanolHCID 67101326HCID 67101326, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9acd0113027c4f55a8ba8e11a538fa16
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932271B2

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