反応 #955953

反応方程式

acetic anhydride

ethyl pyruvate

acetic anhydride

→

ethyl α-acetoxyacrylate

収率 58.5%

溶媒

acetic acid

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   その他to obtain a reaction solution
3. 3
   その他was removed from the reaction solution
4. 4
   workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.)

実験手順

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%).

出典