反应详情

To stirred solution of 2.0 g (0.006 mol) of N-(2-fluorophenyl)-S-methylisothiourea in 50 ml of ethanol was added 2.0 g (0.028 mol) of pyrrolidine and the reaction refluxed for eight hours. The solvent was then evaporated and to the residue was added 100 ml of water and 20 ml of 2 N sodium hydroxide. The aqueous phase was then extracted with ethyl acetate (3×100 ml) and the organic phase dried over magnesium sulphate. Evaporation of the solvent gave a crude residue. This crude residue was then dissolved in 25 ml of hot isopropanol and oxalic acid was added in excess. Upon cooling a white solid crystallized and was collected by filtration and dried at 60° C. for 24 hours to give the oxalate salt of N-(2-fluorophenyl)-1-pyrrolidinecarboximidamide, M.P. 172-173° C.

1. temperaturethe reaction refluxed for eight hours
2. customThe solvent was then evaporated and to the residue
3. additionwas added 100 ml of water and 20 ml of 2 N sodium hydroxide
4. extractionThe aqueous phase was then extracted with ethyl acetate (3×100 ml)
5. dry with materialthe organic phase dried over magnesium sulphate
6. customEvaporation of the solvent
7. customgave a crude residue
8. temperatureUpon cooling a white solid
9. customcrystallized
10. filtrationwas collected by filtration
11. customdried at 60° C. for 24 hours