反应 #955957

ord-506a9d03aa8d4c378f44e32d1cb45819

反应方程式

CC(=O)OC(C)=O
acetic anhydride
CCCCCCCCOC(=O)C(C)=O
octyl pyruvate
CC(=O)OC(C)=O
acetic anhydride
C=C(OC(C)=O)C(=O)OCCCCCCCC
octyl α-acetoxyacrylate
收率 59.2%

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    其他obtaining a second reaction solution
  3. 3
    其他was removed from the second reaction solution
  4. 4
    workup.DISTILLATIONThereafter, the residue was purified by reduced pressure distillation (1 mmHg or less, 80 to 102° C.)

实验过程

Next, in a mixture of the obtained octyl pyruvate (300 g, 1.5 mol) and acetic anhydride (306 g, 3.0 mol), p-toluenesulfonic acid monohydrate (5 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 27 hours, thereby obtaining a second reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (5 mmHg) was removed from the second reaction solution. Thereafter, the residue was purified by reduced pressure distillation (1 mmHg or less, 80 to 102° C.), thereby obtaining octyl α-acetoxyacrylate (215 g, yield 59%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08968975B2uspto-grants-2015_03