反应详情

A mixture of 4-[3-(2,2,2-trifluoroethyl)thioureido]-2-(4-phthalimidobut-2-ynylthio)pyrimidine (0.37 g.), DMF (10 ml.), saturated ethanolic ammonia (1 ml.), EtOH (10 ml.) and yellow mercuric oxide (0.32 g.) was stirred at room temperature for 2 hours and then filtered and the filtrate evaporated to dryness. The residue was treated with EtOH (20 ml.) and 98% hydrazine hydrate (1 ml.) and the mixture heated under reflux for 1 hour and then evaporated to dryness. The residue was stirred with N aqueous HCl and then filtered, The filtrate was basified with 10 N aqueous NaOH and the mixture extracted four times with ether. The combined extracts were dried and evaporated to dryness to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(4-aminobut-2 -ynylthio)pyrimidine (0.17 g.) characterised as the bis hydrogen maleate, m.p. 153°-155° (decomp.)

1. filtrationfiltered
2. customthe filtrate evaporated to dryness
3. additionThe residue was treated with EtOH (20 ml.) and 98% hydrazine hydrate (1 ml.)
4. temperaturethe mixture heated
5. temperatureunder reflux for 1 hour
6. customevaporated to dryness
7. stirringThe residue was stirred with N aqueous HCl
8. filtrationfiltered
9. extractionthe mixture extracted four times with ether
10. customThe combined extracts were dried
11. customevaporated to dryness