تفاعل #63069

معادلة التفاعل

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

3-aminopropanol

sodium hydride

→

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

المردود 47.5%

المذيبات

t-butanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةunder reflux for 4 hours
3. 3
   أخرىevaporated to dryness
4. 4
   أخرىThe residue was partitioned between 2N aqueous acetic acid and ether
5. 5
   استخلاصextracted three times with ether
6. 6
   تجفيفThe combined ether extracts were dried
7. 7
   أخرىevaporated to dryness

الإجراء التجريبي

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.

المصدر