反应详情

5 g of n-Propylamine were added to 2.38 g of 2-[2,6-dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl bromide, and the mixture was stirred at room temperature for 8 hours and then under reflux for 3 hours. The excess of n-propylamine was evaporated. To the residue were added 20 ml of water, 20 ml of a 5% aqueous solution of potassium hydroxide and 100 ml of toluene. The mixture was stirred, and the organic layer was separated, washed with water and dried over anhydrous sodium sulfate. Low-boiling compounds were evaporated under reduced pressure. There were obtained 2.16 g of crude N-{2-[2,6-dichloro-4-(2,2,2-trifluoroethylthio)-phenoxy]-ethyl}-N-(propyl)-amine having a refractive indes of nD20 =1.5210, which were used without further purification) for the preparation of compound No. 1 shown above.

1. temperatureunder reflux for 3 hours
2. customThe excess of n-propylamine was evaporated
3. additionTo the residue were added 20 ml of water, 20 ml of a 5% aqueous solution of potassium hydroxide and 100 ml of toluene
4. stirringThe mixture was stirred
5. customthe organic layer was separated
6. washwashed with water
7. dry with materialdried over anhydrous sodium sulfate
8. customwere evaporated under reduced pressure