反应详情

温度

125 °C

To 4-fluorobenzonitrile (6.1 g) in dry N,N-dimethylformamide (50 mL), under nitrogen, was added 4-mercapto-1,2,3-triazole sodium salt (6.2 g), and the stirred mixture heated in an oil bath at 125° C. for 18 h. The mixture was cooled to room temperature, and most of the solvent stripped at reduced pressure. The residue was partitioned between ethyl acetate and water, the organic phase washed with water, brine, then dried (sodium sulphate), and solvent stripped at reduced pressure. The residue was azeotroped with toluene, and the resulting solid triturated with isohexane, collected by filtration, washed with cold toluene, then isohexane, and dried in vacuo to give the title compound as a yellow solid (8.4 g). 1H NMR (360 MHz, CDCl3) δ 12.45 (1H, br s), 7.92 (1H, s), 7.51 (2H, d, J=8.5 Hz), 7.22 (2H, d, J=8.5 Hz).

1. temperatureThe mixture was cooled to room temperature
2. customThe residue was partitioned between ethyl acetate and water
3. washthe organic phase washed with water, brine
4. dry with materialdried (sodium sulphate), and solvent
5. customThe residue was azeotroped with toluene
6. customthe resulting solid triturated with isohexane
7. filtrationcollected by filtration
8. washwashed with cold toluene
9. dry with materialisohexane, and dried in vacuo