HRID2183537
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
CONDITIONS
反应条件
- 温度
- 125 °C
PROCEDURE
实验过程
A mixture of 7-chloro-5-methyl-3-(2,4,6-trimethyl-phenyl)-pyrazolo[1,5-a]pyrimidine (190 mg, 0.63 mmol) and 1-ethylpropylamine (4 ml) in 1 ml of N-methylpyrrolidinone was heated at 125° C. oil bath for 15 hours. The mixture was quenched with water and extracted with ethyl acetate. The organic layer was dried and concentrated and purified through silica gel column chromatography using chloroform to 2% methanol in chloroform as eluent to give 195 mg (87%) of the title compound as a green solid. 1H NMR (CDCl3) ä 7.87(s, 1H), 6.97(s, 2H), 6.12(d, 1H), 5.85(s, 1H), 3.52(m, 1H), 2.48(s, 3H), 2.09(s, 3H), 2.16(s, 6H), 1.6-1.9(m, 4H), 1.05(t, 6H)ppm.
WORKUP
后处理
- customThe mixture was quenched with water
- extractionextracted with ethyl acetate
- customThe organic layer was dried
- concentrationconcentrated
- custompurified through silica gel column chromatography