反应 #1269826

反应方程式

methacrylic acid 1-ethoxycarbonyl-1,1-difluoro-2-butyl ester

sodium hydroxide

→

methacrylic acid 1-hydroxycarbonyl-1,1-difluoro-2-butyl ester

溶剂

water

反应条件

后处理

1. 1
   其他The reaction liquid
2. 2
   洗涤was washed with 800 g of diisopropyl ether
3. 3
   洗涤The obtained aqueous layer was washed with diluted hydrochloric acid
4. 4
   萃取followed by extraction with diisopropyl ether two times
5. 5
   其他removing water by magnesium sulfate
6. 6
   过滤filtration
7. 7
   workup.DISTILLATIONdistilling diisopropyl ether out

实验过程

A 2 L reactor was charged with 80.0 g (purity 66%), 208 mmol) of methacrylic acid 1-ethoxycarbonyl-1,1-difluoro-2-butyl ester and 80.0 g of water, followed by cooling down to 0° C., adding dropwise 84.8 g (320 mmol/1.5 equivalents) of 15 wt % sodium hydroxide aqueous solution, and stirring at room temperature for 1 hour. The reaction liquid was washed with 800 g of diisopropyl ether. The obtained aqueous layer was washed with diluted hydrochloric acid, followed by extraction with diisopropyl ether two times, removing water by magnesium sulfate, conducting filtration, and distilling diisopropyl ether out, thereby obtaining 15.2 g of the target methacrylic acid 1-hydroxycarbonyl-1,1-difluoro-2-butyl ester.

来源