반응 #722339

반응 방정식

myristic acid

perfluorooctylethanol

toluene

sulfuric acid

→

perfluorooctylethyl myristate

수율 75.0%

용매

water

Acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONwas slowly added
2. 2
   온도The resulting mixture was vigorously refluxed for about 2 hours and 30 minutes
3. 3
   기타was removed azeotropically
4. 4
   기타After completion of the reaction
5. 5
   온도the reaction mixture was cooled
6. 6
   workup.ADDITIONtreated with decoloring carbon
7. 7
   workup.STIRRINGwith stirring
8. 8
   온도cooled to 5° C. to 10° C.
9. 9
   기타followed by crystallization for 1 hour
10. 10
    기타The crystals precipitated
11. 11
    세척to washing
12. 12
    여과filtration with acetonitrile
13. 13
    기타dried

실험 절차

With 500 g of myristic acid were mixed 1,100 g of perfluorooctylethanol and 2,300 ml of toluene, and 20 g of concentrated sulfuric acid was slowly added with stirring. The resulting mixture was vigorously refluxed for about 2 hours and 30 minutes to carry out the reaction until water was removed azeotropically. After completion of the reaction, the reaction mixture was cooled and then treated with decoloring carbon. Acetonitrile was added with stirring and the resulting mixture was ice-cooled to 5° C. to 10° C., followed by crystallization for 1 hour. The crystals precipitated were subjected to washing filtration with acetonitrile and then dried to obtain 1,120 g (yield: 75%) of perfluorooctylethyl myristate.

출처