반응 #476183

반응 방정식

water

Tetrahydrofuran

octane-1,8-diol

diphenylammonium triflate

monochlorobenzene

→

triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate

반응 조건

후처리

1. 1
   기타reaction
2. 2
   기타After completion of the reaction
3. 3
   농축the reaction mixture was concentrated
4. 4
   기타to remove monochlorobenzene
5. 5
   workup.ADDITIONChloroform was added to the concentrate
6. 6
   기타obtained
7. 7
   기타A chloroform layer was separated
8. 8
   세척After repeatedly washing the chloroform layer with ion-exchange water, 4.2 parts of active carbon
9. 9
   workup.ADDITIONwas added to the chloroform layer
10. 10
    기타obtained
11. 11
    여과The chloroform layer was filtered
12. 12
    농축concentrated
13. 13
    기타to obtain pale yellow oily matters
14. 14
    workup.STIRRINGto stir
15. 15
    여과The mixture was filtered
16. 16
    기타the filtrate obtained
17. 17
    농축was concentrated
18. 18
    workup.ADDITIONEthyl acetate was added to the concentrate
19. 19
    기타obtained
20. 20
    농축the residue was concentrated

실험 절차

30.0 parts of TPS-1, 20.0 parts of octane-1,8-diol, 2.2 parts of diphenylammonium triflate and 210 parts of monochlorobenzene were mixed and the resultant mixture was stirred at 80° C. to effect reaction. After completion of the reaction, the reaction mixture was concentrated to remove monochlorobenzene. Chloroform was added to the concentrate obtained and ion-exchanged water was added thereto. A chloroform layer was separated. After repeatedly washing the chloroform layer with ion-exchange water, 4.2 parts of active carbon was added to the chloroform layer obtained to stir for 1 hour. The chloroform layer was filtered and concentrated to obtain pale yellow oily matters. Tetrahydrofuran was added to the oily matters to stir. The mixture was filtered and the filtrate obtained was concentrated. Ethyl acetate was added to the concentrate obtained and the resultant mixture was stirred to conduct decantation. After repeating this operation, the residue was concentrated to obtain 19.5 parts of triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate in the form of pale yellow oil, which is called as TPS-5.

출처