反応 #1269826

反応方程式

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

sodium hydroxide

→

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

溶媒

water

反応条件

後処理

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

実験手順

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.

出典