反应详情

温度

70 °C

A 250 mL round bottom flask was charged with 2,5-difluoro-4-methyoxybenzaldehyde (commercially available from Manchester Organics Ltd., UK) (18.45 g, 107.2 mmol), malonic acid (commercially available from Sigma-Aldrich, St. Louis, Mo., USA) (12.27 g, 117.9 mmol), and 10:1 EtOH/pyridine (27 mL). The mixture was stirred overnight at 70° C. under a reflux condenser and cooled to 0° C. for 2 hours. The precipitated solid was filtered, rinsed with ether, and dried in vacuo to afford H3.1 (16.96 g, 74% yield) as a white powder.

1. temperaturecooled to 0° C. for 2 hours
2. filtrationThe precipitated solid was filtered
3. washrinsed with ether
4. customdried in vacuo
5. customto afford H3.1 (16.96 g, 74% yield) as a white powder