Reaktion #314697

Reaktionsgleichung

2,4-Dibromo-6-methyl-3-nitropyridine

sodium hydrosulfite

sodium hydrosulfite

→

3-amino-2,4-dibromo-6-methylpyridine

Ausbeute 99.0%

Lösungsmittel

methanol

tetrahydrofuran

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGSubsequently, the mixture was stirred for 30 minutes at 65° C
2. 2
   workup.STIRRINGthe mixture was stirred for 30 minutes at 65° C
3. 3
   Temperaturto cool
4. 4
   Extraktionthe mixture was extracted with chloroform
5. 5
   WaschenThe organic layer was washed with saturated brine
6. 6
   Trocknenby drying over sodium sulfate anhydrate
7. 7
   Einengenconcentrating under reduced pressure

Vorschrift

2,4-Dibromo-6-methyl-3-nitropyridine (1.0 g, 3.38 mmol) was dissolved in a mixture of methanol (4 mL) and tetrahydrofuran (6 mL), and a solution of sodium hydrosulfite (3.0 g, 17.23 mmol) in water (7 mL) was added thereto over 5 minutes with stirring at 65° C. Subsequently, the mixture was stirred for 30 minutes at 65° C. To the mixture, a solution of sodium hydrosulfite (3.0 g, 17.23 mmol) in water (7 mL) was further added over 5 minutes, and the mixture was stirred for 30 minutes at 65° C. The resultant mixture was allowed to cool, diluted with water, and then the mixture was extracted with chloroform. The organic layer was washed with saturated brine, followed by drying over sodium sulfate anhydrate and concentrating under reduced pressure, to thereby yield 0.89 g of 3-amino-2,4-dibromo-6-methylpyridine as a colorless solid (yield 99%). The product was crystallized from hexane, to thereby obtain colorless crystals.

Quelle