Dimethyl Sulfate → benzofuran-3-one O-methyl oxime

HRID 612810노트

반응식

HRID 612810 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3](=[N:10][OH:11])[CH2:2]1.[H-].[Na+].S(OC)(O[CH3:18])(=O)=O>O>[CH3:18][O:11][N:10]=[C:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[O:1][CH2:2]1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 73014405Benzofuran-3-one oxime

생성물 1

HCID 54271616benzofuran-3-one O-methyl oxime수율 42%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3.7 g of benzofuran-3-one oxime are dissolved in 15 ml of dimethylfornamide. At 20° C., 1 g of sodium hydride (60%) is added and the mixture is stirred until the evolution of gas ceases. 3.15 g of dimethyl sulphate are then added dropwise and the mixture is stirred at 20° C. for 24 hours. The reaction mixture is poured into water, extracted with ethyl acetate, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. The residue is chromatographed over silica gel using n-hexane/acetone (4:1). 1.7 g (42% of theory) of benzofuran-3-one O-methyl-oxime are obtained as an oil.

후처리

  1. stirringthe mixture is stirred at 20° C. for 24 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. distillationthe solvent is distilled off under reduced pressure
  5. customThe residue is chromatographed over silica gel

출처 및 근거

ORD 기록
ord-1b10c105bb60410db8a8b210609ec1a6
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06005104

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