반응 #1755450

반응 방정식

2,2,3,3-tetrafluoropropan-1-ol

triethylamine

Trifluoromethanesulfonyl fluoride

→

2,2,3,3-tetrafluoropropyl trifluoromethanesulfonate

용매

chloroform

반응 조건

후처리

1. 1
   기타sealed
2. 2
   기타was set to −10° C
3. 3
   기타did not exceed −5° C
4. 4
   workup.ADDITIONOnce the addition
5. 5
   workup.ADDITIONThe reaction mix
6. 6
   세척washed with 2×500 mL portions of water and 1×250 mL portion of 1N HCl
7. 7
   기타The chloroform solvent was removed by rotary evaporation
8. 8
   건조The product was dried over anhydrous magnesium sulfate which
9. 9
   여과was then filtered from the product

실험 절차

2,2,3,3-tetrafluoropropan-1-ol (244.3 g, 1.85 mol, obtained from Sinochem Corp.), triethylamine (187.2 g, 1.85 mol, obtained from Aldrich Chemical Co.) and 500 mL of chloroform were combined in a 2-liter Parr pressure reactor and sealed. The reactor temperature was set to −10° C. Trifluoromethanesulfonyl fluoride (281.33 g, 1.85 mol, obtained from 3M Company) was added at such a rate that the temperature did not exceed −5° C. Once the addition was complete, the mix was held at −10° C. for 45 minutes. The reaction mix was then emptied and washed with 2×500 mL portions of water and 1×250 mL portion of 1N HCl. GC analysis of the reaction mixture indicated a 97 percent conversion to the product. The chloroform solvent was removed by rotary evaporation. The product was dried over anhydrous magnesium sulfate which was then filtered from the product.

출처