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Hydrogen Peroxide → HCID 12850099, 화합물

HRID 973456
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HRID 973456 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH:11]([NH:13][CH2:14][CH:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[C:19]([S:24][CH3:25])[CH:18]=2)[OH:16])[CH3:12])=[CH:5][CH:4]=1.[OH:26]O>CO>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH:11]([NH:13][CH2:14][CH:15]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[C:19]([S:24]([CH3:25])=[O:26])[CH:18]=2)[OH:16])[CH3:12])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 12850096HCID 12850096, 화합물

생성물 1

HCID 12850099HCID 12850099, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 70 ml of methanol was dissolved 2.5 g of α-{[3-(4-methoxyphenyl)-1-methylpropylamino]-methyl}-4-methyl-3-methylthiobenzenemethanol and then 8 ml of an aqueous 30% hydrogen peroxide solution was added dropwise to the solution under ice-cooling. After allowing the reaction mixture to stand overnight the at room temperature, methanol was distilled off and after adding 50 ml of water to the residue, the product was extracted with ethyl acetate. The ethyl acetate layer formed was dried with anhydrous magnesium sulfate and after distilling off the solvent, the residue was purified by a silica gel column chromatography (eluate: a mixture of benzene, ethyl acetate, and methanol (4:3:1 by volume ratio) to provide 2.0 g of the amorphous caramel-like powder of α-{[3-(4-methoxyphenyl)-1-methylpropylamino]methyl}-4-methyl-3-methylsulfinylbenzenemethanol.

후처리

  1. temperaturecooling
  2. distillationthe at room temperature, methanol was distilled off
  3. additionafter adding 50 ml of water to the residue
  4. extractionthe product was extracted with ethyl acetate
  5. customThe ethyl acetate layer formed
  6. dry with materialwas dried with anhydrous magnesium sulfate
  7. distillationafter distilling off the solvent
  8. customthe residue was purified by a silica gel column chromatography (eluate
  9. additiona mixture of benzene, ethyl acetate, and methanol (4:3:1 by volume ratio)

출처 및 근거

ORD 기록
ord-d9557991388e4b538570174d0a04f7af
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05063246

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