Hydrochloric Acid → 3-Bromo-2-methoxypyridin-4-amine

Temperature

0 °C

Methanol (350 mL) was charged in a two-neck RBF equipped with a guard tube and septum and cooled to 0° C. Sodium metal (23 g) was added to it slowly in pieces. After all sodium metal had dissolved, 4-amino-3-bromo-2-chloro pyridine (23 g, 178 mmol) was added and the solution was heated at 180° C. in a pressure vessel for 5-6 h. The reaction mixture was then cooled to 0° C. and adjusted to pH 8 by addition of conc. HCl. Solvent was removed under reduced pressure and the residue was suspended in ethyl acetate. Undissolved impurities were removed by filtration and the filtrate was concentrated under reduced pressure to obtain pure product.

1. customequipped with a guard tube
2. temperaturethe solution was heated at 180° C. in a pressure vessel for 5-6 h
3. temperatureThe reaction mixture was then cooled to 0° C.
4. customSolvent was removed under reduced pressure
5. customwere removed by filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customto obtain pure product

ORD record

ord-a7bc0b78caae469b866cc5ba8b79dc54

Source dataset

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07981891B2