반응 #63072

반응 방정식

4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[3-(3-cyano-2-methylisothioureido)propylthio]pyrimidine

N,N-diethylethylenediamine

→

4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[3-(2-cyano-3-[2-diethylaminoethyl]guanidino)propylthio]pyrimidine

용매

methanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 24 hours
3. 3
   기타evaporated to dryness
4. 4
   workup.ADDITIONWater was added to the residue
5. 5
   추출the mixture extracted with ethyl acetate
6. 6
   추출the ethyl acetate extract
7. 7
   기타dried
8. 8
   기타evaporated to dryness
9. 9
   기타The residue was purified by preparative thin layer chromatography

실험 절차

A mixture of 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[3-(3-cyano-2-methylisothioureido)propylthio]pyrimidine (0.2 g.), N,N-diethylethylenediamine (0.5 ml.) and methanol (2 ml.) was heated under reflux for 24 hours and then evaporated to dryness. Water was added to the residue, the mixture extracted with ethyl acetate and the ethyl acetate extract dried and evaporated to dryness. The residue was purified by preparative thin layer chromatography using ethyl acetate/methanol/ammonia 6:1:0.5 v/v/v as developing solvent to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[3-(2-cyano-3-[2-diethylaminoethyl]guanidino)propylthio]pyrimidine (0.08 g.), characterised as the bis hydrogen maleate, m.p. 76°-80° after recrystallisation from acetone.

출처