تفاعل #476183

معادلة التفاعل

water

Tetrahydrofuran

octane-1,8-diol

diphenylammonium triflate

monochlorobenzene

→

triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate

ظروف التفاعل

المعالجة

1. 1
   أخرىreaction
2. 2
   أخرىAfter completion of the reaction
3. 3
   تركيزthe reaction mixture was concentrated
4. 4
   أخرىto remove monochlorobenzene
5. 5
   workup.ADDITIONChloroform was added to the concentrate
6. 6
   أخرىobtained
7. 7
   أخرىA chloroform layer was separated
8. 8
   غسيلAfter 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
    أخرىobtained
11. 11
    ترشيحThe chloroform layer was filtered
12. 12
    تركيزconcentrated
13. 13
    أخرىto obtain pale yellow oily matters
14. 14
    workup.STIRRINGto stir
15. 15
    ترشيحThe mixture was filtered
16. 16
    أخرىthe filtrate obtained
17. 17
    تركيزwas concentrated
18. 18
    workup.ADDITIONEthyl acetate was added to the concentrate
19. 19
    أخرىobtained
20. 20
    تركيزthe residue was concentrated

الإجراء التجريبي

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.

المصدر