Phosphorus oxychloride → HCID 22258262、化合物

HRID 1610841ノート

反応式

HRID 1610841 の反応式
[C:1]([C:9]1[CH:14]=[CH:13][C:12](=O)[N:11]2[CH:16]=[CH:17][NH:18][C:10]=12)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:21])=O>C1(C)C=CC=CC=1>[Cl:21][C:12]1[N:11]2[CH:16]=[CH:17][N:18]=[C:10]2[C:9]([C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[O:8])=[CH:14][CH:13]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 9964732HCID 9964732、化合物

生成物 1

HCID 22258262HCID 22258262、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.0 g (4.20 mmol) of 8-Benzoylimidazo[1,2-a]pyridin-5(1H)-one (example L, step 2) and 20.0 g (130.44 mmol) of phosphoric trichloride are dissolved in 20 ml toluene and refluxed for 1 h. The solvent is evaporated under vacuum; the crude is dissolved in 200 ml ethyl acetate and extracted with 100 ml saturated sodium hydrogen carbonate solution and 100 ml water. The organic phase is dried over magnesium sulfate, filtrated and concentrated. Petrolether is added to the residue and the precipitate is filtrated to yield 943 mg (87.5% of th.) (5-Chloroimidazo[1,2-a]-pyridin-8-yl)(phenyl)methanone.

後処理

  1. temperaturerefluxed for 1 h
  2. customThe solvent is evaporated under vacuum
  3. dissolutionthe crude is dissolved in 200 ml ethyl acetate
  4. extractionextracted with 100 ml saturated sodium hydrogen carbonate solution and 100 ml water
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. filtrationfiltrated
  7. concentrationconcentrated
  8. additionPetrolether is added to the residue
  9. filtrationthe precipitate is filtrated

出典と根拠

ORDレコード
ord-d0dd206055754426b2099b61da38459b
出典データセット
uspto-grants-2006_01
特許番号
US06984646B2

反応ノート

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