反应详情

温度

70 °C

A mixture of 1-(2-Fluoro-4-nitro-phenyl)-3-methyl-1,2,4-triazole (Intermediate 28) (56.6 g, 0.255 mol) and SnCl22H2O (292 g, 1.29 mol) in ethanol (800 ml) was stirred at 70° C. under N2 for 1 hour. After cooling to room temperature, the reaction mixture was poured onto ice and the pH was made slightly basic by addition of NaHCO3 (solid) and extracted with ethyl acetate (3×). The combined organic phase was washed with brine (2×), dried over sodium sulfate and concentrated in vacuo to give the title compound as a colourless solid (48.8 g).

1. temperatureAfter cooling to room temperature
2. additionthe reaction mixture was poured onto ice
3. extractionextracted with ethyl acetate (3×)
4. washThe combined organic phase was washed with brine (2×)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo