反应详情

温度

135 °C

A mixture of 7-chloro-5-methyl-3-(2,4,6-trimethyl-phenyl)-pyrazolo[1,5-a]pyrimidine (200 mg, 0.66 mmol) and N-propylethylamine (2 ml) in 1 ml of N-methylpyrrolidinone was heated at 135° C. oil bath for 4 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 hexane to 10% ethyl acetate in hexane as eluent to give 150 mg of the title compound as a clear green oil. 1H NMR (CDCl3) ä 6.95(s, 2H), 5.80(s, 1H), 3.85(q, 2H), 3.67(dd, 2H), 2.41(s, 3H), 2.32(s, 3H), 2.21(s, 3H), 2.03(s, 6H), 1.76(m, 2H), 1.29(t, 3H), 0.98(t, 3H) ppm.

1. customThe mixture was quenched with water
2. extractionextracted with ethyl acetate
3. customThe organic layer was dried
4. concentrationconcentrated
5. custompurified through silica gel column chromatography