反应详情

温度

110 °C

A mixture of 4-(4-bromophenylsulphonyl)-1-[2-(2,4-difluorophenyl)ethyl]piperidine (0.38 g, 0.86 mmol), 2-methyl-5-(tributylstannyl)tetrazole (0.64 g, 1.72 mmol) and tetrakis(triphenylphosphine)palladium (100 mg, 0.02 mmol) in DMF was heated at 110° C. for 16 hours while stirring under nitrogen. The solution was poured into water/EtOAc (5/20 ml) and further extracted into EtOAc. The combined organic phase was washed with water, dried (Na2SO4) and evaporated to yield a syrup. Column chromatography (silica, EtOAc) followed by recrystallisation from EtOAc yielded 220 mg of crystalline material. δH (400 MHz, CDCl3) 1.73-1.80 (2H, m), 1.98-2.06 (4H, m), 2.50-2.54 (2H, m), 2.71-2.75 (2H, m), 2.92-2.98 (1H, m), 3.05-3.08 (2H, m), 4.45 (3H, s), 6.71-6.80 (2H, m), 7.09-7.14 (1H, m), 7.99 (1H, d, J 5.2 Hz), 8.34 (1H, d, J 5.2 Hz).

1. extractionfurther extracted into EtOAc
2. washThe combined organic phase was washed with water
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customto yield a syrup
6. customColumn chromatography (silica, EtOAc) followed by recrystallisation from EtOAc