Reaktion #68529

Reaktionsgleichung

HCl

Sodium

sodium

Methanol

4-amino-3-bromo-2-chloro pyridine

→

4-amino-3-bromo-2-methoxypyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a guard tube
2. 2
   Temperaturthe solution was heated at 180° C. in a pressure vessel for 5-6 h
3. 3
   TemperaturThe reaction mixture was then cooled to 0° C.
4. 4
   SonstigeSolvent was removed under reduced pressure
5. 5
   Sonstigewere removed by filtration
6. 6
   Einengenthe filtrate was concentrated under reduced pressure
7. 7
   Sonstigeto obtain pure product

Vorschrift

Methanol (350 mL) was charged in a two-neck round bottom flask 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.

Quelle