反应 #607399
ord-63fc97e5fd3d44d39a240323a87e0b52
反应方程式
3-(4-nitrophenyl)-1-(4-(trifluoromethyl)phenyl)-1H-1,2,4-triazole
→
title compound
收率 77.9%
4-(1-(4-(trifluoromethyl)phenyl)-1H-1,2,4-triazol-3-yl)aniline
收率 77.9%
反应条件
温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度The reaction was cooled to room temperature
- 2过滤filtered through Celite®
- 3洗涤wash
- 4其他The organic layer was separated
- 5浓缩concentrated
- 6其他Purification by flash column chromatography
实验过程
To 3-(4-nitrophenyl)-1-(4-(trifluoromethyl)phenyl)-1H-1,2,4-triazole (22.0 g, 65.8 mmol) in acetic acid (132 mL) and water (110 mL) was added iron powder. The reaction was heated to 90° C. for 18 hours. The reaction was cooled to room temperature and filtered through Celite® followed by an ethyl acetate wash. The organic layer was separated and concentrated. Purification by flash column chromatography using 0-50% ethyl acetate/petroleum ether as eluent provided the title compound as a light yellow solid (15.6 g, 74%): 1H NMR (300 MHz, CDCl3) δ 8.00 (d, J=1.0 Hz, 1H), 7.68-6.92 (m, 6H), 6.29-5.93 (m, 2H), 3.27 (bs, 2H); ESIMS m/z 305 ([M+H]+).