Water → HCID 67200711、化合物

HRID 509975ノート

反応式

HRID 509975 の反応式
C1(S([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([O:19][CH3:20])[CH:18]=[C:13]3[C:12]([CH2:21][C:22]3[CH:23]=[N:24][C:25]([NH:28][CH2:29][C:30]4[C:31]([O:37][CH3:38])=[N:32][CH:33]=[C:34]([F:36])[CH:35]=4)=[N:26][CH:27]=3)=[CH:11]2)(=O)=O)C=CC=CC=1.O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O>O1CCCC1>[F:36][C:34]1[CH:35]=[C:30]([CH2:29][NH:28][C:25]2[N:26]=[CH:27][C:22]([CH2:21][C:12]3[C:13]4[C:14](=[N:15][CH:16]=[C:17]([O:19][CH3:20])[CH:18]=4)[NH:10][CH:11]=3)=[CH:23][N:24]=2)[C:31]([O:37][CH3:38])=[N:32][CH:33]=1

参加物

5

反応物 3

HCID 962WaterHCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 67200202HCID 67200202、化合物

生成物 1

HCID 67200711HCID 67200711、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To [5-(1-benzenesulfonyl-5-methoxy-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyrimidin-2-yl]-(5-fluoro-2-methoxy-pyridin-3-ylmethyl)-amine (125, 1 equivalent) in 15.0 mL of tetrahydrofuran, tetrabutylammonium fluoride trihydrate (2 equivalent) is added. The reaction is stirred at room temperature overnight, then poured into water and extracted with ethyl acetate. The organic layer is dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography eluting with 20-100% ethyl acetate in hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound as a yellow solid.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under vacuum
  5. customThe resulting material is purified by silica gel column chromatography
  6. washeluting with 20-100% ethyl acetate in hexane
  7. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-970d0ecfb0fa4a71ba0a2e877ba066d7
出典データセット
uspto-grants-2015_08
特許番号
US09096593B2

反応ノート

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