반응 #955953
ord-8145e7bb54f94012b03842a0a38f85ab
반응 방정식
acetic anhydride
ethyl pyruvate
acetic anhydride
→
ethyl α-acetoxyacrylate
수율 58.5%
반응 조건
온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONwas added
- 2기타to obtain a reaction solution
- 3기타was removed from the reaction solution
- 4workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.)
실험 절차
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%).