2-Methyl-4-methoxy-5-nitrophenyl mesylate → 2-Methyl-4-methoxy-5-aminophenyl mesylate

HRID 1029998Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1029998
[S:1]([O:5][C:6]1[CH:11]=[C:10]([N+:12]([O-])=O)[C:9]([O:15][CH3:16])=[CH:8][C:7]=1[CH3:17])(=[O:4])(=[O:3])[CH3:2]>[Pd].C(O)C>[S:1]([O:5][C:6]1[CH:11]=[C:10]([NH2:12])[C:9]([O:15][CH3:16])=[CH:8][C:7]=1[CH3:17])(=[O:4])(=[O:3])[CH3:2]

Komponenten

4

Edukt 1

HCID 198211562-Methyl-4-methoxy-5-nitrophenyl mesylate

Produkt 1

HCID 198211482-Methyl-4-methoxy-5-aminophenyl mesylateAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

1.55 g of 10% palladium-on-carbon, 18.8 g (71.9 mmol) of 2-methyl-4-methoxy-5-nitrophenyl mesylate and 120 ml of ethanol were fed into an autoclave (200 ml), and the mixture was then hydrogenated at 50° C. under 50 g/cm2 for 1 hours with stirring. After allowing to cool, palladium-on-carbon was filtered off and the solvent was distilled off under reduced pressure to obtain brown crystals. The crystals thus obtained were recrystallized from ethanol to thereby give 13.4 g (58.2 mmol) of 2-methyl-4-methoxy-5-aminophenyl mesylate in the form of yellow needle-like crystals. The yield was 81%.

Aufarbeitung

  1. temperatureto cool
  2. filtrationpalladium-on-carbon was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. customto obtain brown crystals
  5. customThe crystals thus obtained
  6. customwere recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-721c1db3f9a14e7883e496ee74a8c4fe
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104414

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