反应详情

温度

80 °C

2-(5-Bromopyridin-2-yl)acetic acid hydrochloride (example 42e) (2.34 g, 9.3 mmol) was dissolved in MeOH (18 mL) and conc. H2SO4 (1.5 mL). The mixture was stirred at 80° C. overnight. The solvent was removed under reduced pressure and the mixture was treated with sat. NaHCO3 then extracted with EtOAc, washed with brine, dried over MgSO4, filtered and evaporated to give methyl 2-(5-bromopyridin-2-yl)acetate as a yellow oil (1.97 g, 92%). 1H NMR (400 MHz, dMSO): δ 3.60 (s, 3H), 3.83 (s, 2H), 7.34-36 (d, 1H), 7.99-8.02 (dd, 1H), 8.60-8.61 (d, 1H); MS+H (230, 231).

1. customThe solvent was removed under reduced pressure
2. additionthe mixture was treated with sat. NaHCO3
3. extractionthen extracted with EtOAc
4. washwashed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated