Reaktionsgleichung
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[CH3:9].[N:10]([O-])=O.[Na+].[ClH:14]>>[ClH:14].[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][NH2:10])=[CH:4][C:3]=1[CH3:9]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
4-Bromo-3-methylaniline (10.2 g) was suspended in 6N HCl (85 mL) and cooled to 0° C. A solution of sodium nitrite (4 g in 40 mL H2O) was added over 10 min. The reaction was stirred for 15 min at 0° C. followed by the addition of stannous chloride dihydrate (36 g in 25 mL 12N HCl.) The reaction was stirred for 2 hr at 0° C. The reaction was filtered and the filter cake washed with cold H2O to afford 4-bromo-3-methylphenylhydrazine hydrochloride (Cmpd 9a, 20 g) as a tan solid.
Aufarbeitung
- stirringwas stirred for 2 hr at 0° C
- filtrationThe reaction was filtered
- washthe filter cake washed with cold H2O
Quellen und Nachweise
- ORD-Eintrag
- ord-f46b2edaba374d1191254b7edf33b72d
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07737154B2
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