반응 #1269826

반응 방정식

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

sodium hydroxide

→

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

용매

water

반응 조건

후처리

1. 1
   기타The reaction liquid
2. 2
   세척was washed with 800 g of diisopropyl ether
3. 3
   세척The obtained aqueous layer was washed with diluted hydrochloric acid
4. 4
   추출followed by extraction with diisopropyl ether two times
5. 5
   기타removing water by magnesium sulfate
6. 6
   여과filtration
7. 7
   workup.DISTILLATIONdistilling diisopropyl ether out

실험 절차

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.

출처