5-Fluoro-2-nitroanisole → (3-methoxy-4-nitrophenyl)(methyl)sulfane(WX191877)

HRID 2283508Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2283508
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([O:11][CH3:12])[CH:3]=1.[CH3:13][S-:14].[Na+]>CN(C=O)C.O>[CH3:12][O:11][C:4]1[CH:3]=[C:2]([S:14][CH3:13])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9]

Komponenten

5

Edukt 2

HCID 27792505-Fluoro-2-nitroanisoleHCID 4378561Sodium methanethiolate

Produkt 1

HCID 86688022(3-methoxy-4-nitrophenyl)(methyl)sulfane(WX191877)Ausbeute 59,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 4-fluoro-2-methoxy-1-nitrobenzene (1.38 g, 8.06 mmol) and sodium methyl mercaptide (0.622 g, 8.87 mmol) in DMF (25 mL) was stirred at room temperature for 18 hours. The reaction was the diluted with water and extracted with EtOAc. The combined extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to give (3-methoxy-4-nitrophenyl)(methyl)sulfane (0.95 g, 59%).

Aufarbeitung

  1. extractionextracted with EtOAc
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-86ecef930b4c4432b501cd96b42cc925
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09145402B2

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