Dibenzyl-(4-[1,3]dioxolan-2-yl-2,5-dimethyl-phenyl)amine → HCID 57461076、化合物
反応式
C([N:8](CC1C=CC=CC=1)[C:9]1[CH:14]=[C:13]([CH3:15])[C:12]([CH:16]2[O:20][CH2:19][CH2:18][O:17]2)=[CH:11][C:10]=1[CH3:21])C1C=CC=CC=1>C(O)C.O>[O:17]1[CH2:18][CH2:19][O:20][CH:16]1[C:12]1[C:13]([CH3:15])=[CH:14][C:9]([NH2:8])=[C:10]([CH3:21])[CH:11]=1参加物
4
実験手順
The crude dibenzyl-(4-[1,3]dioxolan-2-yl-2,5-dimethyl-phenyl)amine was dissolved in a 2:1 mixture of ethanol and water (150 mL total) and the resulting mixture was purged with dry nitrogen for 5 minutes. Palladium on carbon (2.3 g, 10 wt. % containing about 50% water) and solid sodium bicarbonate (1.0 g) were added and the resulting mixture was hydrogenated at about 1 atm of hydrogen at 25° C. to 30° C. for about 8 hours. The mixture was then filtered through Celite and the filtrate was concentrated on a rotary evaporator to provide crude 4-[1,3]dioxolan-2-yl-2,5-dimethylphenylamine (5.6 g, 92% yield) as a thick oil. 1H NMR (300 MHz, DMSO-d6) δ 2.05 (s, 3H), 2.22 (s, 3H), 3.7-3.9 (m, 4H), 3.95 (s, 4H), 5.59 (s, 1H), 6.72 (s, 1H), 7.0-7.25 (m, 11H).