反应详情

温度

160 °C

A mixture of 1,2,4-triazole (0.175 g, 2.5 mmol), 4-(4-bromophenylsulphonyl)-1-[2-(2,4-difluorophenyl)ethyl]piperidine (0.54 g, 1.2 mmol), copper bronze (80 mg) and sodium hydride (60%, 100 mg, 2.5 mmol) in NMP (3 ml) was heated under nitrogen at 160° C. for 16 h while stirring. The hot solution was poured into water/CH2Cl2 (10/20 ml) and further extracted into CH2Cl2. The combined organic phase was washed with water, dried (Na2SO4) and evaporated to yield a syrup. Column chromatography [silica, hexane/EtOAc (1:1)] yielded 250 mg of crystalline material. δH (360 MHz, CDCl3) 1.68-1.79 (2H, m), 1.98-2.05 (4H, m), 2.50-2.54 (2H, m), 2.71-2.75 (2H, m), 2.90-2.99 (1H, m), 3.05-3.09 (2H, m), 6.72-6.81 (2H, m), 7.09-7.15 (1H, m), 7.93-8.04 (4H, m), 8.17 (1H, s), 8.72 (1H, s).

1. extractionfurther extracted into CH2Cl2
2. washThe combined organic phase was washed with water
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customto yield a syrup