反应详情

温度

0 °C

To a solution of tert-butyl 4-(6-bromopyridin-2-yl)-4-hydroxypiperidine-1-carboxylate (100 mg) in pyridine (2.5 ml) is added, at 0° C. under argon, POCl3 (0.26 ml). The mixture is stirred at 0° C. and then slowly warmed to room temperature. The mixture is stirred at room temperature overnight. The reaction mixture is subsequently admixed with saturated sodium hydrogencarbonate solution and the aqueous phase is removed. After the aqueous phase has been extracted with tert-butyl methyl ether, the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. The residue is purified by chromatography. This gives tert-butyl 6-bromo-3′,6′-dihydro-2,4′-bipyridine-1′(2′H)-carboxylate (60 mg).

1. temperatureslowly warmed to room temperature
2. stirringThe mixture is stirred at room temperature overnight
3. customthe aqueous phase is removed
4. extractionAfter the aqueous phase has been extracted with tert-butyl methyl ether
5. dry with materialthe combined organic phases are dried over sodium sulphate
6. concentrationconcentrated under reduced pressure
7. customThe residue is purified by chromatography