4-Bromo-2,6-diaminopyridine → HCID 55284821, compound

Temperature

230 °C

A mixture of 1.00 g 2.6-diamino-4-bromopyridine and 0.992 g copper(I)cyanide in 10 ml dimethylformamide was heated under microwave irradiation to 230° C. for 1000 sec. The resulting mixture was partitioned between 10% aqueous ammonium chloride and ethyl acetate. The phases were separated and the aqueous phase was extracted with ethyl acetate. The organic phases were washed with water and brine, dried over magnesium sulfate dihydrate and evaporated. The solid residue was dissolved in hot ethyl acetate and passed through a filter. To the clear mother liquor was added heptane until crystallization started. The mixture was cooled to room temperature and the crystals were collected by filtration to yield 0.528 g of the title compound as yellowish solid.

1. customThe resulting mixture was partitioned between 10% aqueous ammonium chloride and ethyl acetate
2. customThe phases were separated
3. extractionthe aqueous phase was extracted with ethyl acetate
4. washThe organic phases were washed with water and brine
5. dry with materialdried over magnesium sulfate dihydrate
6. customevaporated
7. dissolutionThe solid residue was dissolved in hot ethyl acetate
8. additionTo the clear mother liquor was added heptane
9. customuntil crystallization
10. temperatureThe mixture was cooled to room temperature
11. filtrationthe crystals were collected by filtration

ORD record

ord-718a8f24459a4a108a22572a64afd89f

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08163778B2