Sodium Bicarbonate → HCID 13634839, Verbindung

HRID 1835446Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1835446
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-])=O)[CH:9]=1.C(=O)([O-])O.[Na+]>O1CCCC1.C(O)C.[Pd]>[N:4]1[CH:5]=[CH:6][C:7]([C:8]2[CH:9]=[C:10]([NH2:14])[CH:11]=[CH:12][CH:13]=2)=[CH:2][N:3]=1

Komponenten

6

Edukt 2

HCID 516892Sodium BicarbonateHCID 13634837HCID 13634837, Verbindung

Produkt 1

HCID 13634839HCID 13634839, VerbindungAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A suspension of 3,6dichloro4-(3-nitro-phenyl)pyridazine (0.19 g) and sodium hydrogen carbonate (147 mg) in tetrahydrofuran (2 ml) and ethanol (5 ml) was hydrogenated over palladium on carbon (10% w/w, 50% wet, 100 mg) under hydrogen atmosphere for 3 hours. The catalyst was filtered off, and the filtrate was evaporated. The residue was diluted with ethyl acetate and an aqueous solution of sodium hydrogen carbonate. The separated organic layer was washed with brine and dried over potassium carbonate. The organic layer was evaporated under reduced pressure to give 3-(pyridazin-4-yl)phenylamine (106 mg, 88.3%).

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. additionThe residue was diluted with ethyl acetate
  4. washThe separated organic layer was washed with brine
  5. dry with materialdried over potassium carbonate
  6. customThe organic layer was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-508a0c27b2fe4ff98a11ae341c533faa
Quelldatensatz
uspto-grants-2004_08
Patentnummer
US06770667B1

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