反应详情

A mixture of 15.0 mL water and 11.0 mL concentrated sulfuric acid was added to 13.0 g of 4,4'-dinitro-2-aminobiphenyl, and the resulting mixture was stirred for 2 hours while heating, whereupon 26.5 g of crushed ice was added. On an ice bath, an aqueous solution of 3.51 g of sodium nitrite was added dropwise to the aforementioned mixture; the resulting system was mixed for 10 minutes and subsequently allowed to stand at quiescence for several minutes. The reaction mixture was then added dropwise to a boiling solution that had been prepared by adding 33.4 mL concentrated sulfuric acid to 25 mL of water. Boiling was continued for 5 minutes, after which the mixture was poured into a beaker on an ice bath. The filter cake afforded by suction filtration was purified by column chromatography to give 10.9 g of 4,4'-dinitro-2-hydroxybiphenyl as a yellowish brown powder.

1. additionwas added
2. additionthe resulting system was mixed for 10 minutes
3. waitto stand at quiescence for several minutes
4. additionThe reaction mixture was then added dropwise to a boiling solution that
5. customhad been prepared
6. waitBoiling was continued for 5 minutes
7. additionafter which the mixture was poured into a beaker on an ice bath
8. customThe filter cake afforded by suction filtration
9. customwas purified by column chromatography