반응 #65845

반응 방정식

pyrocatechol

triethylamine

2,3-dichloro-1,1,1,4,4,4-hexafluorobut-2-ene

→

2-(1-Chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.DISTILLATION1200 ml of the solvent were then distilled off under vacuum
2. 2
   추출The product was extracted with diethyl ether
3. 3
   세척the organic phase was washed twice with 10% by Weight aqueous sodium hydroxide solution and once with water
4. 4
   건조After drying over magnesium sulphate
5. 5
   농축the solution was concentrated
6. 6
   workup.DISTILLATIONsubjected to fractional distillation under vacuum

실험 절차

110 g of pyrocatechol were dissolved in 1500 ml of acetonitrile, and 200 g of triethylamine were added. 235 g of 2,3-dichloro-1,1,1,4,4,4-hexafluorobut-2-ene were added dropwise to the mixture at 75° C. The reaction mixture was subsequently stirred for 2 hours at 75° C. 1200 ml of the solvent were then distilled off under vacuum and the residue was taken up in 1500 ml of water. The product was extracted with diethyl ether and the organic phase was washed twice with 10% by Weight aqueous sodium hydroxide solution and once with water. After drying over magnesium sulphate, the solution was concentrated and subjected to fractional distillation under vacuum. The yield was 258 g (=84% of theory). The boiling point was 63° C. at 12 mbar. The NMR spectra showed the following characteristic absorptions: 19F NMR: -66.8 and -79.7 ppm. 1H NMR: 4.71 ppm.

출처