反応 #63069

反応方程式

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

3-aminopropanol

sodium hydride

→

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

収率 47.5%

溶媒

t-butanol

反応条件

後処理

1. 1
   温度heated
2. 2
   温度under reflux for 4 hours
3. 3
   その他evaporated to dryness
4. 4
   その他The residue was partitioned between 2N aqueous acetic acid and ether
5. 5
   抽出extracted three times with ether
6. 6
   乾燥The combined ether extracts were dried
7. 7
   その他evaporated to dryness

実験手順

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.

出典