反应详情

To a suspension of 3-(pyridin-3-yl)acrylic acid (1.03 g, 6.9 mmol) in DCM (25 ml) is added oxalyl chloride (2 M in DCM, 17.25 mL, 34.5 mmol) dropwise. With stir, 100 uL of DMF is added and the mixture is stirred at RT for 30 min then heat at reflux for 3 h. The solvent is removed under vacuum and ether is added (40 mL). The suspension is stirred at RT for 30 min then filtered. The solid is washed with ether (20 mL) and dried under vacuum to give the tilted compound as a white solid. (1.22 g, 87%).

1. stirringthe mixture is stirred at RT for 30 min
2. temperaturethen heat
3. temperatureat reflux for 3 h
4. customThe solvent is removed under vacuum and ether
5. additionis added (40 mL)
6. stirringThe suspension is stirred at RT for 30 min
7. filtrationthen filtered
8. washThe solid is washed with ether (20 mL)
9. customdried under vacuum