Phosphorus oxychloride → HCID 22258262, 화합물

HRID 1610841노트

반응식

HRID 1610841 반응식
[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

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 9964732HCID 9964732, 화합물

생성물 1

HCID 22258262HCID 22258262, 화합물수율 87.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0dd206055754426b2099b61da38459b
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06984646B2

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