Hydrochloric Acid → 2-Chloro-1-(6-chloropyridin-2-YL)ethanone
反応式
[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]=1参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-2b5d1454342e4719acf4d5a437d30dd9
- 出典データセット
- uspto-grants-1995_02
- 特許番号
- US05387710
反応ノート
読み込み中…