Water → 6-Bromo-2-methoxypyridin-3-amine

A solution of 2-methoxypyridin-3-amine (39.4 g) in N,N-dimethylformamide (200 mL) was cooled to −30° C., and a solution of N-bromosuccinimide (62.1 g) in N,N-dimethylformamide (100 mL) was added dropwise. After stirring for 30 minutes, the reaction solution was poured into water and extracted with chloroform. The organic layer was sequentially washed with a saturated sodium sulfite solution, water and brine and dried over sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→4:1) to give 6-bromo-2-methoxypyridin-3-amine as a yellow powder (51.9 g, 80%).

1. extractionextracted with chloroform
2. washThe organic layer was sequentially washed with a saturated sodium sulfite solution, water and brine
3. dry with materialdried over sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→4:1)

ORD-Eintrag

ord-1f69f2bc68bc4c5eb7d97fee0c8c7ec9

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08822503B2