Nitrogen → HCID 44185547, 화합물

HRID 2387566노트

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HRID 2387566 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]([OH:14])=[O:13])[C:6]([CH3:15])=[CH:5]2.[C:16]1([S:22]([C:25]2[CH:32]=[CH:31][CH:30]=[CH:29][C:26]=2[CH:27]=O)(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[CH2:33]([SiH](CC)CC)[CH3:34].FC(F)(F)C(O)=O.N#N.C(=O)([O-])O.[Na+]>ClCCl>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]([O:14][CH2:33][CH3:34])=[O:13])[C:6]([CH3:15])=[C:5]2[CH2:27][C:26]1[CH:29]=[CH:30][CH:31]=[CH:32][C:25]=1[S:22]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:24])=[O:23]

참가 물질

8

반응물 6

HCID 947NitrogenHCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 516892Sodium BicarbonateHCID 6409162-(Phenylsulfonyl)benzaldehydeHCID 674666192(5-fluoro-2-methyl-1H-indol-1-yl)acetic acid

생성물 1

HCID 44185547HCID 44185547, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2(5-fluoro-2-methyl-1H-indol-1-yl)acetic acid (1.29 g, 1.49 mmol), 2-(phenylsulfonyl)benzaldehyde (1.50 g, 6.10 mmol) and triethylsilane (4.30 ml, 27.0 mmol) in dichloromethane (40 ml) was added trifluoroacetic acid (1.25 ml, 16.5 mmol) dropwise under N2 at 0° C. over 30 minutes. The reaction was warmed to room temperature and stirred for 2 hours. Saturated aqueous sodium hydrogen carbonate solution was added and the product extracted with dichloromethane. The combined organic extracts were washed with saturated brine, dried over MgSO4 and concentrated in vacuo giving a brown oil which was triturated with petroleum ether (40-60° C.) to give a white solid (1.34 g, 2.88 mmol 52%).

후처리

  1. extractionthe product extracted with dichloromethane
  2. washThe combined organic extracts were washed with saturated brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customgiving a brown oil which
  6. customwas triturated with petroleum ether (40-60° C.)
  7. customto give a white solid (1.34 g, 2.88 mmol 52%)

출처 및 근거

ORD 기록
ord-96feebdf09ae4bd08e7c4f53e5e68ac0
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268878B2

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