反应详情

The product (300 g) of Step 1 and p-methoxyphenol (2 g) was added to a 2 l. round bottom flask fitted with a thermometer, condenser, stirrer and inlet for nitrogen, and containing acetonitrile (1000 ml) and anhydrous potassium carbonate (330 g). The reaction mixture was stirred under reflux for 8 hours and cooled, and the salts were filtered off. The filtrate was evaporated under reduced pressure to remove the solvent, and the residue was dissolved in dichloromethane. The solution was dried (Na2SO4), filtered and evaporated. Distillation of the residue afforded n-butyl 2-bromoacrylate (196 g; 90%), b.p. 90°/15 mmHg.

1. customround bottom flask fitted with a thermometer, condenser, stirrer and inlet for nitrogen
2. temperatureunder reflux for 8 hours
3. temperaturecooled
4. filtrationthe salts were filtered off
5. customThe filtrate was evaporated under reduced pressure
6. customto remove the solvent
7. dissolutionthe residue was dissolved in dichloromethane
8. dry with materialThe solution was dried (Na2SO4)
9. filtrationfiltered
10. customevaporated
11. distillationDistillation of the residue