反应详情

温度

100 °C

To a 2-Amino-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 6-tert-butyl ester 3-ethyl ester (5.0 g, 15 mmol) in DMF (50 mL) solution was added formamidine acetate (2.39 g, 23 mmol, 1.5 equiv). The mixture was heated at 100° C. in an oil bath for overnight. The reaction mixture was cooled to rt and then concentrated in vacuo. Ethyl acetate (50 mL) was added to the reaction solid mixture and stirred at rt for 2 h. The mixture was then filtered, rinsed with ethyl acetate (25 mL). The solid was placed in a vacuum oven and dried for overnight to yield a white solid (4.17 g, 90.6%). 1H NMR (CD3OD-d4) δ 8.05 (s, 1H), 4.57 (s, 2H), 3.61 (t, 2H), 2.92 (t, 2H), 1.42 (s, 9H); LCMS RT=2.78 min, [M+H]+=308.0.

1. temperatureThe reaction mixture was cooled to rt
2. concentrationconcentrated in vacuo
3. additionEthyl acetate (50 mL) was added to the reaction solid mixture
4. filtrationThe mixture was then filtered
5. washrinsed with ethyl acetate (25 mL)
6. customdried for overnight