반응 #63069

반응 방정식

4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-methylsulphonylpyrimidine

3-aminopropanol

sodium hydride

→

4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(3-aminopropyloxy)pyrimidine

수율 47.5%

용매

t-butanol

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도under reflux for 4 hours
3. 3
   기타evaporated to dryness
4. 4
   기타The residue was partitioned between 2N aqueous acetic acid and ether
5. 5
   추출extracted three times with ether
6. 6
   건조The combined ether extracts were dried
7. 7
   기타evaporated to dryness

실험 절차

4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-methylsulphonylpyrimidine (0.15 g.) was added to a mixture of 3-aminopropanol (0.075 g.), t-butanol (5 ml.) and a 50% w/w dispersion of sodium hydride in mineral oil (0.05 g.) which was stirred under an argon atmosphere. The mixture was stirred at room temperature for 2 hours, heated under reflux for 4 hours and then evaporated to dryness. The residue was partitioned between 2N aqueous acetic acid and ether, and the aqueous phase basified with 17N NaOH and extracted three times with ether. The combined ether extracts were dried and evaporated to dryness to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(3-aminopropyloxy)pyrimidine (0.07 g.) which was used without further purification.

출처