反应详情

7.4 ml of fuming nitric acid was slowly added to 92.1 ml of acetic acid under ice-cooling, followed by stirring for 10 minutes, and a solution of 52.1 ml of acetic anhydride containing 25 g of 3-bromothiophene was slowly added in such a manner that the bulk temperature did not exceed 10° C., followed by stirring at 10 ° C. for 2 hours. Ice was added to the reaction solution, and the resulting crystals were collected by filtration, and washed with water and diethyl ether/n-hexane=1/5 successively, to give 17.4 g of the title compound.

1. temperaturecooling
2. customdid not exceed 10° C.
3. stirringby stirring at 10 ° C. for 2 hours
4. additionIce was added to the reaction solution
5. filtrationthe resulting crystals were collected by filtration
6. washwashed with water and diethyl ether/n-hexane=1/5 successively