Hydrochloric Acid → HCID 21862775, compound

4.68 g of the β-piperidinostyrene/diethyl phthalate mixture were dissolved in 70 ml of anhydrous tetrahydrofuran, and 1.01 g (10 mmol) of triethylamine were added to the resulting solution. 2.60 g (12 mmol) of 4-fluorophenacyl bromide were then added to the resulting mixture, which was then stirred at room temperature for 3 hours. At the end of this time, 30 ml of 1N aqueous hydrochloric acid were added to the reaction mixture, and the mixture was stirred at room temperature for a further 1 hour. It was then extracted with diethyl ether. The organic extract was washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure and the residue was applied to a silica gel chromatography column and eluted with a 95:5 by volume mixture of hexane and ethyl acetate, to give 0.50 g of the title compound as a slightly yellow oily substance.

1. stirringthe mixture was stirred at room temperature for a further 1 hour
2. extractionIt was then extracted with diethyl ether
3. extractionThe organic extract
4. washwas washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was then removed by distillation under reduced pressure
7. washeluted with a 95:5 by volume mixture of hexane and ethyl acetate

ORD record

ord-954569f93add4143b7444e345a44f33a

Source dataset

uspto-grants-1999_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05908858