反应详情

In 100 ml of methanol was dissolved 20.5 g of 4-cyanobenzoic acid t-butyl ester and 13.9 g of hydroxylamine. To the solution was added, while stirring at room temperature, 128 g of triethylamine; The resulting mixture was stirred for one hour at 85° C. then concentrated under reduced pressure. The concentrate was dissolved in ethyl acetate, and the solution was washed with water. The organic layer was concentrated under reduced pressure to give a crude product, which was recrystallized from isopropyl ether to afford 11.45 g of the title compound as a colorless crystalline product.

1. additionTo the solution was added
2. stirringThe resulting mixture was stirred for one hour at 85° C.
3. concentrationthen concentrated under reduced pressure
4. dissolutionThe concentrate was dissolved in ethyl acetate
5. washthe solution was washed with water
6. concentrationThe organic layer was concentrated under reduced pressure
7. customto give a crude product, which
8. customwas recrystallized from isopropyl ether