HRID54951
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 3-(4-fluorophenyl)-2-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (100 mg), triethylamine (0.4 ml) and acetic anhydride (0.2 ml) in dry 1,2-dichloroethane (3 ml) was refluxed for 2 days. The reaction mixture was cooled and concentrated in vacuo. The residue was dissolved in dichloromethane and the solution was washed with an aqueous saturated sodium bicarbonate solution and brine, dried and concentrated in vacuo. The residue was purified by column chromatography on silica gel and the obtained oil was crystallized from diisopropyl ether to give 4-acetyl-3-(4-fluorophenyl)-2-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (60 mg).
WORKUP
后处理
- temperaturewas refluxed for 2 days
- temperatureThe reaction mixture was cooled
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in dichloromethane
- washthe solution was washed with an aqueous saturated sodium bicarbonate solution and brine
- customdried
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography on silica gel
- customthe obtained oil was crystallized from diisopropyl ether