반응 #65304

반응 방정식

water

2,2-bis(4-hydroxyphenyl)hexafluoropropane

5-chloro-2-nitrobenzotrifluoride

sodium carbonate

→

(4-(4-nitro-3-trifluoromethylphenoxy)phenyl]hexafluoropropane

수율 95.9%

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타After the reaction
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The organic layer was washed with water
4. 4
   건조dried on anhydrous sodium sulfate
5. 5
   여과After filtration
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   기타to recover a crude product, which
8. 8
   기타was then purified by silica gel column chromatography (eluent: toluene/hexane=1/1)
9. 9
   workup.ADDITIONtreated by activated carbon

실험 절차

16.0 g (47.6 mmol) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane, 26.9 g (119 mmol) of 5-chloro-2-nitrobenzotrifluoride and 20.2 g (190 mmol) of sodium carbonate were reacted at 150° C. for 4 hours in 100 ml of dimethylformamide. After the reaction, the product was injected into 250 ml of iced water and extracted with ethyl acetate. The organic layer was washed with water and dried on anhydrous sodium sulfate. After filtration, the solvent was distilled off to recover a crude product, which was then purified by silica gel column chromatography (eluent: toluene/hexane=1/1) and then treated by activated carbon to obtain 32.6 g (yield: 95.9%) of 2,2-bis[(4-(4-nitro-3-trifluoromethylphenoxy)phenyl]hexafluoropropane.

출처