反应详情

To a stirred solution of 25.0 parts of 2,2,2-trifluoroethanol in 175 parts of N,N-diethylethanamine were added portionwise 62.2 parts of 2-naphthalenesulfonyl chloride. Upon completion, a mixture of 1.5 parts of N,N-dimethyl-4-pyridinamine and 25 parts of ethyl acetate was added during a period of 20 minutes. Upon complete addition, stirring was continued overnight at room temperature. The reaction mixture was filtered and the filtrate was evaporated in vacuo. The residue was stirred in water and solidified product was filtered off under reduced pressure. The precipitated product was dissolved in dichloromethane. The organic layer was dried, filtered and evaporated in vacuo. The residue was treated with petroleum ether. After filtration, the precipitated product was crystallized from 2-propanol. The product was filtered off and dried, yielding 65.3 parts (89%) of 2,2,2-trifluoroethyl 2-naphthalenesulfonate; mp. 72.7° C. (int. 36).

1. additionwas added during a period of 20 minutes
2. additionUpon complete addition
3. filtrationThe reaction mixture was filtered
4. customthe filtrate was evaporated in vacuo
5. stirringThe residue was stirred in water
6. filtrationsolidified product was filtered off under reduced pressure
7. dissolutionThe precipitated product was dissolved in dichloromethane
8. customThe organic layer was dried
9. filtrationfiltered
10. customevaporated in vacuo
11. additionThe residue was treated with petroleum ether
12. filtrationAfter filtration
13. customthe precipitated product was crystallized from 2-propanol
14. filtrationThe product was filtered off
15. customdried