反应详情

Crotonyl chloride (7 ml) was added to a solution of 2,4-dichloro-6-nitrophenol (10.3 g) in methylene chloride (20 ml) and the mixture was heated under reflux for 12 hours. The solution was diluted with further methylene chloride (200 ml) and extracted several times with a 10% sodium hydroxide solution. The organic layer was washed with water dried (Na2SO4) and the solvent removed under reduced pressure to give a pale brown oil which crystallised on standing for 24 hours 2,4-dichloro-6-nitrophenyl crotonate melted at <60°.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 12 hours
3. extractionextracted several times with a 10% sodium hydroxide solution
4. washThe organic layer was washed with water
5. dry with materialdried (Na2SO4)
6. customthe solvent removed under reduced pressure
7. customto give a pale brown oil which
8. customcrystallised