反应详情

A mixture of 4-[3-(2,2,2-trifluoroethyl)thioureido]-[(3-phthalimido)propylthio]pyrimidine (0.4 g.), N,N,-dimethylformamide (5 ml.), saturated ethanolic ammonia (10 ml.) and yellow mercuric oxide (280 mg.) was stirred at room temperature for 3 hours and then filtered and the filtrate evaporated to dryness. A solution of the residue in ethanol (10 ml.) was treated with hydrazine hydrate (1 ml.), the mixture heated under reflux for 1 hour and then evaporated to dryness. The residue was stirred with 1 N hydrochloric acid and then filtered and the filtrate basified with 17 N NaOH. The mixture was extracted with ether and the combined ether extracts dried and evaporated to dryness to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[(3-amino)propylthio]-pyrimidine which was used without further purification.

1. filtrationfiltered
2. customthe filtrate evaporated to dryness
3. additionA solution of the residue in ethanol (10 ml.) was treated with hydrazine hydrate (1 ml.)
4. temperaturethe mixture heated
5. temperatureunder reflux for 1 hour
6. customevaporated to dryness
7. stirringThe residue was stirred with 1 N hydrochloric acid
8. filtrationfiltered
9. extractionThe mixture was extracted with ether
10. dry with materialthe combined ether extracts dried
11. customevaporated to dryness