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

HRID 1059905

반응식

HRID 1059905 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-85ffa0499c814ce1bfe6c4a830ea5708
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521643B1

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