Reaktion #955953
ord-8145e7bb54f94012b03842a0a38f85ab
Reaktionsgleichung
acetic anhydride
ethyl pyruvate
acetic anhydride
→
ethyl α-acetoxyacrylate
Ausbeute 58.5%
Lösungsmittel
Reaktionsbedingungen
Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas added
- 2Sonstigeto obtain a reaction solution
- 3Sonstigewas removed from the reaction solution
- 4workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.)
Vorschrift
First, to a mixture of ethyl pyruvate (315 g, 2.7 mol) and acetic anhydride (554 g, 5.4 mol), p-toluenesulfonic acid monohydrate (8 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 24 hours to obtain a reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (40 to 50 mmHg) was removed from the reaction solution. Thereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.) to obtain ethyl α-acetoxyacrylate (250 g, yield 58%).