反応 #524792

反応方程式

Crotonyl chloride

2,4-dichloro-6-nitrophenol

→

2,4-dichloro-6-nitrophenyl crotonate

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux for 12 hours
3. 3
   抽出extracted several times with a 10% sodium hydroxide solution
4. 4
   洗浄The organic layer was washed with water
5. 5
   乾燥dried (Na2SO4)
6. 6
   その他the solvent removed under reduced pressure
7. 7
   その他to give a pale brown oil which
8. 8
   その他crystallised

実験手順

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°.

出典