反应 #1365741

反应方程式

hydrochloric acid

4-mercaptopyrimidine

1-(3-chloropropyl)-4-(3-trifluoromethylphenyl)piperazine

triethylamine

→

product

收率 59.0%

4-[3-(4-{3-Trifluoromethylphenyl}piperazinyl)propylthio]pyrimidine

收率 59.0%

溶剂

DMF

反应条件

后处理

1. 1
   萃取extracted with MTB ether
2. 2
   萃取extracted with ethyl acetate
3. 3
   干燥the organic phase was dried over MgSO4
4. 4
   浓缩concentrated
5. 5
   其他The residue was purified by chromatography (mobile phase: CH2Cl2/CH3OH=98/2)

实验过程

1.5 g (13.4 mmol) of 4-mercaptopyrimidine, 4.3 g (14 mmol) of 1-(3-chloropropyl)-4-(3-trifluoromethylphenyl)piperazine and 1.5 g (15 mmol) of triethylamine in 5 ml of DMF were stirred at 100° C. for 1 hour. The mixture was then poured into 5% strength hydrochloric acid and extracted with MTB ether. The aqueous phase was made alkaline with sodium hydroxide solution and then extracted with ethyl acetate, and the organic phase was dried over MgSO4 and concentrated. The residue was purified by chromatography (mobile phase: CH2Cl2/CH3OH=98/2). 3.0 g of product were obtained as a yellowish oil (=59% yield).

来源