tert-Butoxy bis(dimethylamino)methane → HCID 1473179、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[C:13]([C:14]#[N:15])=[C:12]([CH3:16])[O:11][N:10]=1.C(O[CH:22](N(C)C)[N:23]([CH3:25])[CH3:24])(C)(C)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[C:13]([C:14]#[N:15])=[C:12](/[CH:16]=[CH:22]/[N:23]([CH3:25])[CH3:24])[O:11][N:10]=1参加物
4
実験手順
To a solution of 1.5 g (6.3389 mmol) 3-(2-chloro-6-fluorophenyl)-5-methylisoxazole-4-carbonitrile in 100 mL dry toluene, were added 2.10 g (12.6779 mmol) tert-Butoxy-bis(dimethylamino)methane. The reaction mixture was heated under reflux for 12 h. The mixture was concentrated in vacuo and was dried in the high vacuum. Petroleum ether was added to the crystallized residue. The product was collected by filtration and 1.791 g (yield of theory: 95.9%) of clean product were obtained. Result of LC/MS MH+: 292.0; 1H NMR (DMSO-d6; CCl4): 2.93 (3H, s, N—CH3), 3.17 (3H, s, N—CH3), 5.15-5.20 (1H, d, C2H2), 7.74-7.78 (1H, d, C2H2), 7.45-7.52 (1H, dd, CH-arom.), 7.57-7.59 (1H, d, CH-arom.), 7.65-7.71 (1H, d, CH-arom.)