反应详情

温度

180 °C

A mixture of 2,4-difluorobenzoyl chloride (88.3 g) and 4-nitroaniline (32.9 g) was heated at 180° C. for 25 minutes. Zinc chloride (39 g) was added portionwise to the resulting mixture. The mixture was stirred for 2.5 hours at 195° C. and cooled to 130° C. To the mixture was added 3N hydrochloric acid (100 ml) and the resulting mixture was refluxed for 2 hours, then the supernatant was decanted out. 75% Sulfuric acid was added to the residue and the mixture was stirred at 130° C. for 2 hours. The reaction mixture was poured into ice and extracted with dichloromethane. The organic layer was washed with 3N hydrochloric acid (600 ml), 3N sodium hydroxide (1 l), and water successively, dried, and evaporated. The solid residue (15 g) was recrystallized from ethanol to give crystals of 2-amino-5-nitro-2',4'-difluorobenzophenone (6.3 g).

1. temperaturecooled to 130° C
2. temperaturethe resulting mixture was refluxed for 2 hours
3. customthe supernatant was decanted out
4. addition75% Sulfuric acid was added to the residue
5. stirringthe mixture was stirred at 130° C. for 2 hours
6. additionThe reaction mixture was poured into ice
7. extractionextracted with dichloromethane
8. washThe organic layer was washed with 3N hydrochloric acid (600 ml), 3N sodium hydroxide (1 l), and water successively
9. customdried
10. customevaporated
11. customThe solid residue (15 g) was recrystallized from ethanol