Phosphorus oxychloride → 2-Chloroimidazo[1,2-a]pyridine-3-sulfonyl chloride

반응식

[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][N:5]2[C:10]=1[S:11]([OH:14])(=O)=[O:12].P(Cl)(Cl)([Cl:17])=O>>[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][N:5]2[C:10]=1[S:11]([Cl:17])(=[O:14])=[O:12]

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 144224132-Chloroimidazo[1,2-a]pyridine-3-sulfonic acid

생성물 1

HCID 108579162-Chloroimidazo[1,2-a]pyridine-3-sulfonyl chloride

실험 절차

2-Chloroimidazo[1,2-a]pyridine-3-sulfonic acid (5.0 g) is suspended in 30 ml of phosphorus oxychloride and refluxed for 5 hours. After cooling, the reaction solution is poured into 250 ml of ice water and extracted with dichloromethane. The dichloromethane layer is collected, dried on anydrous sodium sulfate and then concentrated to dryness under reduced pressure to afford 4.6 g of the title compound as pale yellowish crystals.

후처리

temperaturerefluxed for 5 hours
temperatureAfter cooling
extractionextracted with dichloromethane
customThe dichloromethane layer is collected
dry with materialdried on anydrous sodium sulfate
concentrationconcentrated to dryness under reduced pressure

출처 및 근거

ORD 기록: ord-b91dec64a93c49ad9f6f4b6bc3ccd85c
출처 데이터셋: uspto-grants-1991_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05017212

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