反应详情

温度

10 °C

To a 500 mL flask was charged 95 g (0.34 mole) of 2-(4-chlorophenyl-2-[(1,2,4-triazol-1-yl)methyl]butyramide and 95 g (0.97 mole) of 95% sulfuric acid and 95 g of ice. The reaction was stirred at reflux for 55 hours, after which the reaction was cooled to 10° C. and partitioned between ethyl acetate and water. The mixture was treated with 200 g of 10% sodium hydroxide which resulted in a pH 10 aqueous phase. The organic phase was extracted with 200 g of water, then 200 g of 10% sodium hydroxide and again with 200 mL of water The aqueous phases were combined and washed with ethyl ether then acidified to pH 5 at which point a solid formed. The solid was filtered, washed with water, dried and gave 73 g (77% yield) of a white solid, melting point 182°-184° C.

1. temperatureat reflux for 55 hours
2. custompartitioned between ethyl acetate and water
3. additionThe mixture was treated with 200 g of 10% sodium hydroxide which