反应 #320757

反应方程式

cyclopentylamine

triethylamine

5,7 Dichloro-6-(4-methylphenyl)-1,2,4-triazolo-[1,5-a]pyrimidine

→

5-chloro-6-(4-methylphenyl)-7-cyclopentylamino-1,2,4-triazolo[1,5-a]pyrimidine

收率 87.0%

溶剂

tetrahydrofuran

tetrahydrofuran

反应条件

后处理

1. 1
   其他(20° C.)
2. 2
   其他The reaction mixture was then evaporated in vacuo
3. 3
   萃取the residue extracted with dichloromethane and water (100 ml each)
4. 4
   干燥The organic layer was dried over sodium sulphate
5. 5
   其他the solvent evaporated in vacuo
6. 6
   其他The residue was crystallized from ethyl acetate

实验过程

5,7 Dichloro-6-(4-methylphenyl)-1,2,4-triazolo-[1,5-a]pyrimidine (1.8 g, 6 mmol) was dissolved in tetrahydrofuran. A solution of cyclopentylamine (0.51 g, 6 mmol) and triethylamine (0.61 g, 6 mmol) in tetrahydrofuran (2 ml) was then added with stirring and the stirring continued for a further 3 hours at ambient temperature (20° C.). The reaction mixture was then evaporated in vacuo and the residue extracted with dichloromethane and water (100 ml each). The organic layer was dried over sodium sulphate and the solvent evaporated in vacuo. The residue was crystallized from ethyl acetate to give 1.7 g 5-chloro-6-(4-methylphenyl)-7-cyclopentylamino-1,2,4-triazolo[1,5-a]pyrimidine as yellowish crystals, m.pt. 158° C. Yield: 87% of theoretical 1H-NMR: δ=1.3-1.75 (2 m, 8H); 2.43(s,1H); 3.73 (m,1H); 5.97 (d,1H); 7.25 (m,4H); 8.25(s,1H) ppm

来源