反应详情

A suspension of 96.0 g. of aluminum chloride and 135 ml. of methylene chloride is stirred and treated with a mixture of 60 ml. of methylene chloride, 63 ml. of acetyl chloride, and 77.4 g. of 2-nitrobiphenyl. The mixture is heated at reflux for three hours and cautiously poured into 1200 g. of ice and 900 ml. of concentrated hydrochloric acid. The mixture is extracted with methylene chloride. The extract is washed with water and aqueous sodium bicarbonate, dried (Na2SO4), and the solvent removed to give a dark oil. This is stirred with 200 ml. of ether and the resulting solid recovered and washed with 1:1 ether:Skellysolve B; yield 53.50 g., m.p. 106°-109°. For analysis a sample is recrystallized from ether; m.p. 108°-111°.

1. additionA suspension of 96.0 g
2. additiontreated with a mixture of 60 ml
3. temperatureThe mixture is heated
4. temperatureat reflux for three hours
5. additioncautiously poured into 1200 g
6. extractionThe mixture is extracted with methylene chloride
7. washThe extract is washed with water and aqueous sodium bicarbonate
8. dry with materialdried (Na2SO4)
9. customthe solvent removed
10. customto give a dark oil
11. customof ether and the resulting solid recovered
12. washwashed with 1:1 ether
13. customFor analysis a sample is recrystallized from ether