反应详情

10 ml of 30% aqueous hydrogen peroxide is heated to 35–40° C. 20 ml of acetic anhydride is added dropwise under cooling, so that the temperature does not exceed 40–50° C. 0.02 g of wolframic acid is added and the reaction mixture is stirred for 0.5 hours at 50–55° C. 3 grams of the amide (7) is added to the mixture portionwise and the reaction mixture is stirred for 6 hours at 50–55° C. The suspension is then cooled to 20–25° C. and poured, under stirring, into 100 ml of cold (0–5° C.) water. The suspension is stirred for 30 minutes and the solid is filtered off, washed by water and dried at 40–50° C. Yield: 2.44 g (76.5%).

1. temperatureunder cooling, so that the temperature
2. customdoes not exceed 40–50° C
3. stirringthe reaction mixture is stirred for 6 hours at 50–55° C
4. temperatureThe suspension is then cooled to 20–25° C.
5. additionpoured
6. stirringThe suspension is stirred for 30 minutes
7. filtrationthe solid is filtered off
8. washwashed by water
9. customdried at 40–50° C