反応 #1269827

反応方程式

1-chloro-1-methylcyclopentane

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

THF

triethylamine

→

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

収率 83.0%

溶媒

water

反応条件

後処理

1. 1
   workup.STIRRINGby stirring at 0° C. for 20 minutes
2. 2
   workup.ADDITIONwas added
3. 3
   抽出followed by extraction two times with diisopropyl ether
4. 4
   その他removing water by magnesium sulfate
5. 5
   ろ過a filtration
6. 6
   workup.DISTILLATIONdistilling diisopropyl ether out

実験手順

A 2 L reactor was charged under nitrogen with 7.0 g (purity 78%, 25 mmol) of methacrylic acid 1-hydroxycarbonyl-1,1-difluoro-2-butyl ester and 300 mL of THF (dehydrated), followed by cooling down to 0° C., adding 6.5 mL (47 mmol/1.9 equivalents) of triethylamine, and stirring at 0° C. for 10 minutes. Then, furthermore 4.7 g (40.0 mmol/1.6 equivalents) of 1-chloro-1-methylcyclopentane was added, followed by stirring at 0° C. for 20 minutes. To the reaction liquid 500 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 6.6 g of the target methacrylic acid 1-(1-methylcyclopentyloxycarbonyl)-1,1-difluoro-2-butyl ester. Upon this, purity was 96%, and yield was 83%.

出典