Ammonium formate → HCID 18943538、化合物
反応式
[F:1][C:2]([F:20])([F:19])[C:3]([N:5]1[CH2:11][CH2:10][C:9]2[CH:12]=[C:13]([N+:16]([O-])=O)[CH:14]=[CH:15][C:8]=2[CH2:7][CH2:6]1)=[O:4].C([O-])=O.[NH4+]>C1COCC1>[NH2:16][C:13]1[CH:14]=[CH:15][C:8]2[CH2:7][CH2:6][N:5]([C:3](=[O:4])[C:2]([F:20])([F:1])[F:19])[CH2:11][CH2:10][C:9]=2[CH:12]=1参加物
4
実験手順
Into a 500 ml round bottomed flask, the product from step (b) (17 g) and ammonium formate (17 g) in THF (250 ml) were added. To the nitrogen purged reaction mixture, 10% Pd—C (4 g) was added. The reaction mixture was stirred at reflux for 3 hours. The reaction mixture was allowed to cool to room temperature and filtered through celite. The filtrate was diluted with water (200 ml) and extracted with EtOAc (3×). The combined EtOAc extracts were washed with saturated NaHCO3, brine, dried over NaSO4, and solvent evaporated in vacuo to give the sub-title compound as an off-white solid (12.9 g). 1H NMR (300 MHz, DMSO-d6) δ 6.83-6.78 (m, 1H); 6.39-6.31 (m, 2H); 4.91 (s, 2H); 3.66-3.56 (m, 4H); 2.81-2.73 (m, 4H); MS: ESI (positive): 259 (M+H).