反应详情

A solution of 9.7 g of 5-tert-butylsalicylic acid and 7.6 g of 2-methyl-4-nitroaniline in 120 ml of xylene is heated at 65° to 70° C. To a reaction solution is added a solution of 2.6 g of phosphorus trichloride in 30 ml of xylene. The whole mixture is refluxed for 2 hours. The hot reaction solution is decanted. The supernatant solution is cooled on an ice bath. The crystalline precipitate is collected by filtration. Recrystallization from methanol gives 11.5 g of the title compound as pale yellow needles, melting at 202°-204° C.

1. temperatureThe whole mixture is refluxed for 2 hours
2. customThe hot reaction solution is decanted
3. temperatureThe supernatant solution is cooled on an ice bath
4. filtrationThe crystalline precipitate is collected by filtration
5. customRecrystallization from methanol