Sodium Dithionite → 2,4-Dibromo-6-methylpyridin-3-amine

Temperatur

65 °C

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.

1. stirringSubsequently, the mixture was stirred for 30 minutes at 65° C
2. stirringthe mixture was stirred for 30 minutes at 65° C
3. temperatureto cool
4. extractionthe mixture was extracted with chloroform
5. washThe organic layer was washed with saturated brine
6. dry with materialby drying over sodium sulfate anhydrate
7. concentrationconcentrating under reduced pressure

ORD-Eintrag

ord-2e4c9183f7d14226a1e0acca1bad3866

Quelldatensatz

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07560547B2