反应详情

In a 200 mL flask, benzyl 4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)benzylcarbamate (0.599 g, 1.28 mmol) was suspended in hydrogen bromide in acetic acid (33 wt %, 8.00 mL, 45.7 mmol). The suspension was stirred vigorously at room temperature for 1 hour. To the resulting suspension was added diethyl ether (100 mL), and the reaction mixture was stirred for 30 minutes at room temperature. The resulting precipitate was collected via filtration and treated with sodium hydroxide (1 N) and extracted with ethyl acetate (3×75 mL). The combined organic layers were dried over magnesium sulfate, filtered, and concentrated to give the title compound as a white solid (0.395 g, 92% yield): 1H NMR (400 MHz, DMSO-d6) δ 9.45 (s, 1H), 8.25-8.03 (m, 4H), 7.74-7.62 (m, 2H), 7.60-7.48 (m, 2H), 3.85 (s, 2H); 19F NMR (376 MHz, DMSO-d6) δ −56.97; ESMIS m/z 318 ([M+H]+) (—NH2).

1. stirringthe reaction mixture was stirred for 30 minutes at room temperature
2. filtrationThe resulting precipitate was collected via filtration
3. additiontreated with sodium hydroxide (1 N)
4. extractionextracted with ethyl acetate (3×75 mL)
5. dry with materialThe combined organic layers were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated