Malonic Acid → (E)-3-(2,5-difluoro-4-methoxy-phenyl)-acrylic acid
반응식
[F:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([F:12])=[CH:6][C:3]=1[CH:4]=O.C(O)(=O)[CH2:14][C:15]([OH:17])=[O:16]>CCO.N1C=CC=CC=1>[F:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([F:12])=[CH:6][C:3]=1/[CH:4]=[CH:14]/[C:15]([OH:17])=[O:16]참가 물질
4
반응 조건
- 온도
- 70 °C
실험 절차
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.