3,5-dibroMo-2-Methoxypyridin-4-aMine synthesis

Yield:1393563-12-6 32.4 g

Reaction Conditions:

with N-Bromosuccinimide in acetic acid at 10 - 35; for 3 h;

Steps:

28.1 (1)
Synthesis of 3,5-dibromo-2-methoxypyridin-4-amine

(1)
Synthesis of 3,5-dibromo-2-methoxypyridin-4-amine
A mixture of 2-methoxy-pyridin-4-ylamine (15 g) and NBS (47.3 g) was stirred in an acetic acid solvent (150 mL) at room temperature for three hours.
The reaction mixture was concentrated under reduced pressure, and a 5 M aqueous sodium hydroxide solution (200 mL) was added to the residue at 0° C., followed by extraction with diethyl ether.
The organic layer was directly purified by a silica gel pad (ethyl acetate/n-heptane, 10%) to give the title compound (32.4 g).
ESI-MS m/z 283 [M+H]⁺

References:

US2013/143907,2013,A1 Location in patent:Paragraph 0418; 0419