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Sodium Dithionite → 4-Methoxy-3-methylsulfanylmethyl-phenylamine

HRID 47440
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인쇄 미리보기

반응식

HRID 47440 반응식
S(S([O-])=O)([O-])=O.[Na+].[Na+].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][C:12]=1[CH2:20][S:21][CH3:22].C(=O)([O-])O.[Na+]>CO.O>[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][C:12]=1[CH2:20][S:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24489Sodium DithioniteHCID 516892Sodium BicarbonateHCID 227451381-Methoxy-2-methylsulfanylmethyl-4-nitrobenzene

생성물 1

HCID 227451794-Methoxy-3-methylsulfanylmethyl-phenylamine수율 33.5%

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

Sodium dithionite (3.264 g) was added to a solution of 1-methoxy-2-methylsulfanylmethyl-4-nitro-benzene (0.8 g), and sodium hydrogen carbonate (1.57 g) in methanol:water (1:1, 200 ml) and stirred at room temperature for 16 h. Solvent was removed at reduced pressure, the residue partitioned between water and ethyl acetate, the organic phase separated, washed with brine dried (Na2SO4) and solvent removed at reduced pressure to give the title compound (0.23 g) as a brown oil. m/z (API+): 184 (MH+).

후처리

  1. customSolvent was removed at reduced pressure
  2. customthe residue partitioned between water and ethyl acetate
  3. customthe organic phase separated
  4. washwashed with brine
  5. dry with materialdried (Na2SO4) and solvent
  6. customremoved at reduced pressure

출처 및 근거

ORD 기록
ord-7eb1f9319b0a402c825caf499aa87c8f
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06699879B1

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