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4-Nitrophenyl methyl sulfide → (Rs)-s-methyl-s-(4-nitrophenyl)-n-tosylsulphimide

HRID 548957
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HRID 548957 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N-:11]Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.O.O.O.[Na+].[CH3:17][S:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1>C(#N)C.C(OCC)(=O)C>[CH3:17][S:18]([C:19]1[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=1)=[N:11][S:8]([C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][CH:4]=1)(=[O:10])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 961094-Nitrophenyl methyl sulfideHCID 517414chloramine-T trihydrate

생성물 1

HCID 59683178(Rs)-s-methyl-s-(4-nitrophenyl)-n-tosylsulphimide수율 22%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

10.0 g (35.3 mmol) of chloramine-T trihydrate (Aldrich) are added to 5.0 g (29.6 mmol) of 1-methylsulphanyl-4-nitrobenzene in 120 ml of acetonitrile at room temperature. The mixture is stirred at room temperature for 4 hours and then diluted with ethyl acetate. The mixture is filtered with suction and the filter cake is washed with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated. The resulting residue is recrystallized from methanol. 2.2 g (6.5 mmol; yield: 22%) of the product are obtained.

후처리

  1. filtrationThe mixture is filtered with suction
  2. washthe filter cake is washed with ethyl acetate
  3. dry with materialThe combined organic phases are dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is recrystallized from methanol
  7. custom2.2 g (6.5 mmol; yield: 22%) of the product are obtained

출처 및 근거

ORD 기록
ord-46e8fd89e72b42cfa50550d8d73a9ec4
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943629B2

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