Sulfuryl chloride → 2-Chloro-1-(4-methylpyridin-2-yl)propan-1-one

HRID 1059905

反応式

HRID 1059905 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8](=[O:11])[CH2:9][CH3:10])[CH:3]=1.S(Cl)([Cl:15])(=O)=O>C(Cl)(Cl)Cl>[Cl:15][CH:9]([CH3:10])[C:8]([C:4]1[CH:3]=[C:2]([CH3:1])[CH:7]=[CH:6][N:5]=1)=[O:11]

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 186309841-(4-Methylpyridin-2-yl)propan-1-one

生成物 1

HCID 186674842-Chloro-1-(4-methylpyridin-2-yl)propan-1-one

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a stirred solution of 1-(4-methylpyridin-2-yl)propan-1-one (0.9 g) in chloroform (5 ml) was added a solution of sulfuryl chloride (0.533 ml) in chloroform (5 ml) dropwise. The resultant mixture was refluxed for 2 hours and evaporated under reduced pressure. The pH was adjusted to 8.5 with a saturated aqueous sodium hydrogencarbonate solution, and the mixture was extracted with ethyl acetate twice. The combined organic layer was washed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, n-hexane:dichloromethane=1:1) to give 2-chloro-1-(4-methylpyridin-2-yl)propan-1-one (0.71 g).

後処理

  1. customevaporated under reduced pressure
  2. extractionthe mixture was extracted with ethyl acetate twice
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography (silica gel 25 g, n-hexane:dichloromethane=1:1)

出典と根拠

ORDレコード
ord-85ffa0499c814ce1bfe6c4a830ea5708
出典データセット
uspto-grants-2003_02
特許番号
US06521643B1

関連ノート

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