反应详情

温度

100 °C

A 10M solution of Methylamine in H2O (30.0 mL, 386 mmol) was added to a stainless steel reactor containing 3-amino-6-bromopyridine-2-carboxylic acid ethyl ester (Compound 6E, 7.614 g, 31.07 mmol) in MeOH (20.0 mL). The reactor was sealed and heated to 100° C. for 16 hours. The cooled reaction mixture was transferred to a round bottom flask and concentrated in vacuo forming a yellow precipitate which was collected by filtration. Further precipitate formed in the filtrate which was also collected. The combined precipitates were dried in vacuo to afford the title compound as 6.18 g of a yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.80 (br. s., 1H), 7.27 (d, J=8.6 Hz, 1H), 6.91 (d, J=8.6 Hz, 1H), 6.02 (br. s., 2H), 2.97 (d, J=5.1 Hz, 3H).

1. customThe reactor was sealed
2. customThe cooled reaction mixture
3. customwas transferred to a round bottom flask
4. concentrationconcentrated in vacuo
5. customforming a yellow precipitate which
6. filtrationwas collected by filtration
7. customFurther precipitate formed in the filtrate which
8. customwas also collected
9. customThe combined precipitates
10. customwere dried in vacuo