反应详情

A mixture of 100 parts by volume of phosphorus trichloride and 40 parts of 2,8-bis-(trifluoromethyl)-4-hydroxyquinoline is refluxed for 8 hours. Most of the excess phosphorus trichloride is then distilled off, the residue is poured onto 200 parts of ice-water and the pH is brought to 12-13 with 12 N sodium hydroxide solution. The mixture is then extracted with methylene chloride, the extract is dried over sodium sulfate and the solvent is stripped off under reduced pressure. 40.2 parts=94% of theory of 2,8-bis-(trifluoromethyl)-4-chloroquinoline of melting point 40°-42° C. are obtained.

1. temperatureis refluxed for 8 hours
2. distillationMost of the excess phosphorus trichloride is then distilled off
3. additionthe residue is poured onto 200 parts of ice-water
4. extractionThe mixture is then extracted with methylene chloride
5. dry with materialthe extract is dried over sodium sulfate