反应详情

Thionyl chloride (1,000 g, 8.4 m) was then added to the 2-chloro-4-nitrobenzamide (200 g, 1 m) while the mixture was warmed. After addition, the mixture was refluxed for approximately three hours. The excess thionyl chloride was removed by distillation leaving a reaction mixture residue. Benzene (500 ml) was added to the cold reaction mixture residue to extract the reaction product. The extract was washed with diluted sodium hydroxide solution and water until neutralized and then dried over anhydrous sodium sulfate. The benzene solvent was distilled off and the reaction product was crystallized from methanol to yield 2-chloro-4-nitrobenzonitrile (145 g, 79%, mp 73°-75° C.).

1. temperaturewas warmed
2. additionAfter addition
3. temperaturethe mixture was refluxed for approximately three hours
4. customThe excess thionyl chloride was removed by distillation
5. customleaving a reaction mixture residue
6. extractionto extract the reaction product
7. washThe extract was washed with diluted sodium hydroxide solution and water until neutralized and
8. dry with materialthen dried over anhydrous sodium sulfate
9. distillationThe benzene solvent was distilled off
10. customthe reaction product was crystallized from methanol