Hydrochloric Acid → 2-Chloro-1-(6-chloropyridin-2-YL)ethanone
반응식
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[N:5]=1)(=[O:3])[CH3:2].Cl.S(Cl)([Cl:15])(=O)=O>O1CCOCC1>[Cl:10][C:6]1[N:5]=[C:4]([C:1]([CH2:2][Cl:15])=[O:3])[CH:9]=[CH:8][CH:7]=1참가 물질
5
실험 절차
A solution of 2-acetyl-6-chloropyridine (7.48 g) in 1,4-dioxane (112 ml) was added 4N hydrogen chloride in 1,4-dioxane (12.6 ml). To the solution, sulfuryl chloride (13.51 ml) was added dropwise at 30° C. After stirring for 0.5 hour, ice water (150 ml) was added to the solution and the organic layer was separated, washed with brine, dried over anhydrous sodium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel with a mixture of n-hexane and toluene (1:1) as an eluent to give chloromethyl 6-chloro-2-pyridyl ketone (7.05 g) as a powder.
후처리
- customthe organic layer was separated
- washwashed with brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated in vacuo
- customThe residue was purified by column chromatography on silica gel with a mixture of n-hexane and toluene (1:1) as an eluent
출처 및 근거
- ORD 기록
- ord-2b5d1454342e4719acf4d5a437d30dd9
- 출처 데이터셋
- uspto-grants-1995_02
- 특허 번호
- US05387710
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