反应详情

10 gms of 5-(4-Fluoro-phenyl)-5-oxo-pentanoic acid and 5.6 gms of triethyl amine was added to 25 ml of toluene. 5.1 gms of Pivollyl chloride was added and stirred the reaction mass at room temperature for about 2 hours. 4 ml of Morpholine in 25 ml of toluene was added to the reaction mass at 0° C. Stirred the reaction mass for about 30 minutes at 0-5° C. and 20 ml of water was added. To the reaction mass 30 ml of brine solution was added and organic layer was separated. Dried the separated organic layer over sodium sulfate. Distill off the solvent completely under reduced pressure at 50-55° C. The resulted oily mass was dissolved in 12 ml of toluene and 60 ml of hexane. Cooled the reaction mass and 12 ml of toluene was added. Stirred the reaction mass for about 1-2 hours at 0-5° C., filtered, washed with 5 ml of hexane and dried at 40-45° C. to get 10 gms of 1-(4-Fluoro-phenyl)-5-morpholin-4-yl-pentane-1,5-dione.

1. stirringStirred the reaction mass for about 30 minutes at 0-5° C.
2. customorganic layer was separated
3. dry with materialDried the separated organic layer over sodium sulfate
4. distillationDistill off the solvent completely under reduced pressure at 50-55° C
5. dissolutionThe resulted oily mass was dissolved in 12 ml of toluene
6. temperatureCooled the reaction mass and 12 ml of toluene
7. additionwas added
8. stirringStirred the reaction mass for about 1-2 hours at 0-5° C.
9. filtrationfiltered
10. washwashed with 5 ml of hexane
11. customdried at 40-45° C.