反应详情

温度

22.5 °C

3.74 ml (45.65 mmol) of oxalyl chloride were added drop wise to a suspension of 10 g (41.8 mmol) of 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylic acid in ml of anhydrous THF, at 20-25° C. and under nitrogen atmosphere. When the addition of oxalyl chloride was concluded, the mixture was stirred at 20-25° C. for 4 h. Afterwards, the resulting mixture was diluted with 50 ml of anhydrous THF, followed by the distillation of 15 ml at 35-40° C. under vacuum, in order to remove the remaining HCl. The reaction was cooled to 20-25° C. and 8 g (149.57 mmol) of ammonium chloride were added followed by addition of 20 ml of 8% aqueous solution of sodium bicarbonate. After further addition of 8.8 g (104.97 mmol) of sodium bicarbonate, the mixture was left under powerful stirring over 4 h at 20-25° C. To conclude with, the suspension was filtered and washed twice with 50 ml of a saturated aqueous sodium bicarbonate solution and twice with 50 ml of water The solid was dried on a vacuum drier at 50° C. to yield 5.6 g (56.2%) of 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxamide as Form R-5.

1. customat 20-25° C.
2. distillationfollowed by the distillation of 15 ml at 35-40° C. under vacuum, in order
3. customto remove the remaining HCl
4. temperatureThe reaction was cooled to 20-25° C.
5. waitthe mixture was left
6. stirringunder powerful stirring over 4 h at 20-25° C
7. filtrationwas filtered
8. washwashed twice with 50 ml of a saturated aqueous sodium bicarbonate solution and twice with 50 ml of water The solid
9. customwas dried on a vacuum drier at 50° C.