反応 #791931

反応方程式

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

溶媒

ethyl acetate

toluene

water

反応条件

後処理

1. 1
   温度The mixture is cooled
2. 2
   workup.ADDITIONdiluted
3. 3
   抽出extracted three times
4. 4
   乾燥The organic phase is dried over magnesium sulphate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 1:9)

実験手順

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).

出典