Nitrogen → HCID 44185547、化合物

HRID 2387566ノート

反応式

HRID 2387566 の反応式
[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]

参加物

8

反応物 6

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

生成物 1

HCID 44185547HCID 44185547、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-96feebdf09ae4bd08e7c4f53e5e68ac0
出典データセット
uspto-grants-2012_09
特許番号
US08268878B2

反応ノート

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