반응 #1269828

반응 방정식

1-chloro-1-ethylcyclopentane

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

THF

triethylamine

→

methacrylic acid 1-(1-ethylcyclopentyloxycarbonyl)-1,1-difluoro-2-butyl ester

수율 83.0%

용매

water

반응 조건

후처리

1. 1
   workup.STIRRINGby stirring at 0° C. for 20 minutes
2. 2
   workup.ADDITIONwas added
3. 3
   추출followed by extraction two times with diisopropyl ether
4. 4
   기타removing water by magnesium sulfate
5. 5
   여과a filtration
6. 6
   workup.DISTILLATIONdistilling diisopropyl ether out

실험 절차

A 2 L reactor was charged under nitrogen with 5.6 g (purity 78%, 20.0 mmol) of methacrylic acid 1-hydroxycarbonyl-1,1-difluoro-2-butyl ester and 240 mL of THF (dehydrated), followed by cooling down to 0° C., adding 5.2 mL (37.6 mmol/1.9 equivalents) of triethylamine, and stirring at 0° C. for 10 minutes. Then, furthermore 14.24 g (3.2 mmol/1.6 equivalents) of 1-chloro-1-ethylcyclopentane was added, followed by stirring at 0° C. for 20 minutes. To the reaction liquid 800 mL of water was added, followed by extraction two times with diisopropyl ether, removing water by magnesium sulfate, conducting a filtration, and distilling diisopropyl ether out, thereby obtaining 5.52 g of the target methacrylic acid 1-(1-ethylcyclopentyloxycarbonyl)-1,1-difluoro-2-butyl ester. Upon this, purity was 96%, and yield was 83%.

출처