Reaktion #791931

Reaktionsgleichung

hydrochloric acid

compound

2-(4-Fluorophenyl)-5-methyl-1-phenyl-hexane-1,4-dione

N-amino-hexahydroazepine

dimethylformamide

→

3-(4-Fluorophenyl)-1-hexahydroazepinyl-5-isopropyl-2-phenyl-pyrrole

Lösungsmittel

ethyl acetate

toluene

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is cooled
2. 2
   workup.ADDITIONdiluted
3. 3
   Extraktionextracted three times
4. 4
   TrocknenThe organic phase is dried over magnesium sulphate
5. 5
   Einengenconcentrated in vacuo
6. 6
   Sonstigethe residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 1:9)

Vorschrift

1.7 ml of conc. hydrochloric acid are added to 5 g (16.7 mmol) of the compound from Example 2 and 5.7 g (50.1 mmol) of N-amino-hexahydroazepine in 100 ml of toluene AR and 80 ml of dimethylformamide and the mixture is boiled in a water separator for 24 hours. The mixture is cooled, diluted using 200 ml of ethyl acetate and extracted three times using 1N hydrochloric acid and twice using saturated sodium hydrogen carbonate solution. The organic phase is dried over magnesium sulphate and concentrated in vacuo, and the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 1:9).

Quelle