反应详情

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 2 N aqueous acetic acid and ether, and the aqueous phase basified with 17 N 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.

1. temperatureheated
2. temperatureunder reflux for 4 hours
3. customevaporated to dryness
4. customThe residue was partitioned between 2 N aqueous acetic acid and ether
5. extractionextracted three times with ether
6. dry with materialThe combined ether extracts were dried
7. customevaporated to dryness