反応 #476183

反応方程式

water

Tetrahydrofuran

octane-1,8-diol

diphenylammonium triflate

monochlorobenzene

→

triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate

反応条件

後処理

1. 1
   その他reaction
2. 2
   その他After completion of the reaction
3. 3
   濃縮the reaction mixture was concentrated
4. 4
   その他to remove monochlorobenzene
5. 5
   workup.ADDITIONChloroform was added to the concentrate
6. 6
   その他obtained
7. 7
   その他A chloroform layer was separated
8. 8
   洗浄After 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
    その他obtained
11. 11
    ろ過The chloroform layer was filtered
12. 12
    濃縮concentrated
13. 13
    その他to obtain pale yellow oily matters
14. 14
    workup.STIRRINGto stir
15. 15
    ろ過The mixture was filtered
16. 16
    その他the filtrate obtained
17. 17
    濃縮was concentrated
18. 18
    workup.ADDITIONEthyl acetate was added to the concentrate
19. 19
    その他obtained
20. 20
    濃縮the residue was concentrated

実験手順

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.

出典