Potassium Hydroxide → CID 87191335

HRID 2089002

反応式

HRID 2089002 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10](S(C3C=CC=CC=3)(=O)=O)[CH:9]=2)[CH:5]=[C:4]([Cl:26])[N:3]=1.[OH-].[K+]>C(O)C.O>[Cl:26][C:4]1[CH:5]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[NH:10][CH:9]=2)[CH:7]=[C:2]([Cl:1])[N:3]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 866498693-(2,6-dichloropyridin-4-yl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 87191335CID 87191335収率 88.3%

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

反応条件

温度
40 °C

実験手順

To a solution of Example 7a (5.72 g, 15 mmol) in 60 mL ethanol/water (5/1) was added powdered KOH (2 g, 35 mmol). The resulting solution was heated at 40° C. for 2 hours. Most of the solvent was removed in vacuo, and the residue was diluted with ethyl acetate. A solid was filtered from the material and discarded. The organics were washed with water, brine, dried over MgSO4, filtered, and concentrated. The crude material was triturated with dichloromethane and filtered, giving 3.5 g of the title compound as a white solid. MS (ESI+) m/z 263.6 (M+H)+.

後処理

  1. customMost of the solvent was removed in vacuo
  2. additionthe residue was diluted with ethyl acetate
  3. filtrationA solid was filtered from the material
  4. washThe organics were washed with water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude material was triturated with dichloromethane
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-dbe488fa85d8415a9d7ac19307942f55
出典データセット
uspto-grants-2013_05
特許番号
US08435980B2

関連ノート

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