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 2N 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 2N 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