6-Isocyanato-2,2,4,4-tetrefluoro-1,3-benzodioxene → HCID 59252134、化合物
反応式
[CH:1]1[C:6]([N:7]=[C:8]=[O:9])=[CH:5][C:4]2[C:10]([F:17])([F:16])[O:11][C:12]([F:15])([F:14])[O:13][C:3]=2[CH:2]=1.[CH3:18][O:19][C:20]([C:22]1[CH:27]=[C:26]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([NH2:35])[CH:30]=2)[CH:25]=[CH:24][N:23]=1)=[O:21]>C(Cl)Cl>[F:14][C:12]1([F:15])[O:13][C:3]2[CH:2]=[CH:1][C:6]([NH:7][C:8]([NH:35][C:31]3[CH:30]=[C:29]([CH:34]=[CH:33][CH:32]=3)[O:28][C:26]3[CH:25]=[CH:24][N:23]=[C:22]([C:20]([O:19][CH3:18])=[O:21])[CH:27]=3)=[O:9])=[CH:5][C:4]=2[C:10]([F:16])([F:17])[O:11]1参加物
4
実験手順
To a stirring solution of 2,2,4,4-tetrafluoro-6-isocyanato-1,3-benzodioxene (0.816 g, 3.28 mmol) was added 4-(3-aminophenoxy)pyridine-2-carboxylic acid methyl ester (0.800 g, 3.28 mmol) in DCM (13 mL) in portions. The homogenous contents turned white and opaque within 1 min. of addition, and were allowed to stir at room temperature for 12 h. The heterogenous mixture was filtered, and solid product repeatedly washed with DCM to remove residual starting material. The desired product was collected as a white powder, 1.36 g (83%). 1H-NMR (DMSO-d6) δ 9.08 (d, 2H), 8.59 (s, 1H), 8.07 (s, 1H), 7.60 (dd, 1H), 7.37 (m, 4H), 7.25 (d, 1H), 7.20 (dd, 1H), 6.80 (d, 1H), 3.82 (s, 3H); MS LC MS [M+H]+=494.1, RT=3.23 min.