Phosphorus oxychloride → 4-Chloro-3-phenylthieno[2,3-b]pyridine

HRID 215990ノート

反応式

HRID 215990 の反応式
[C:1]1([C:7]2[C:15]3[C:14](=O)[CH:13]=[CH:12][NH:11][C:10]=3[S:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:14]1[CH:13]=[CH:12][N:11]=[C:10]2[S:9][CH:8]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:15]=12

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 684349933-phenyl-7H-thieno[2,3-b]pyridine-4-one

生成物 1

HCID 684343754-Chloro-3-phenylthieno[2,3-b]pyridine

実験手順

3-Phenyl-7H-thieno[2,3-b]pyridine-4-one (0.7 g, 4.29 mmol) was added to phosphorous oxychloride (10 ml) and heated to reflux for 4 hr. The solvent was removed to near dryness and the residue dissolved in DCM. The solution was washed with water followed by saturated sodium hydrogen carbonate and dried over magnesium sulfate. The solution was filtered through a pad of silica and solvents removed in vacuo to give 4-chloro-3-phenyl-thieno[2,3-b]pyridine. Yield=0.261 g (25%).

後処理

  1. temperatureheated
  2. temperatureto reflux for 4 hr
  3. customThe solvent was removed
  4. dissolutionthe residue dissolved in DCM
  5. washThe solution was washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationThe solution was filtered through a pad of silica and solvents
  8. customremoved in vacuo

出典と根拠

ORDレコード
ord-0ccbab9c684d488a88ddde1f0c9f8bee
出典データセット
uspto-grants-2012_06
特許番号
US08193215B2

反応ノート

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