反应详情

2.1 g (10.1 mmol) 2-(4-Aminophenyl)-2-phenylacetonitrile (prepared by catalytic hydrogenation of phenylcyanomethylenequinone oxime according to the method of R. B. Davis, D. D. Carlos, G. S. Mattingly, J. Org. Chem. 1965, 30, 2607) and 1.8 g (9.9 mmol) 7-Chloro-5-ethylpyrazolo[1,5-a]pyrimidine (Example 1, Step B) were dissolved in 50 ml dry ethanol and heated with reflux for 10 h. Solid materials, which precipitated after cooling to room temperature, were filtered, the filtrate evaporated in vacuo, the residue treated with 10% aqueous sodium carbonate solution, and extracted with dichloromethane. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo to afford the crude title compound as an oil, which was pure enough for the next step as detected by its 1H-NMR spectrum.

1. temperatureheated
2. temperaturewith reflux for 10 h
3. customSolid materials, which precipitated
4. filtrationwere filtered
5. customthe filtrate evaporated in vacuo
6. additionthe residue treated with 10% aqueous sodium carbonate solution
7. extractionextracted with dichloromethane
8. dry with materialThe organic layer was dried over sodium sulfate
9. customthe solvent was removed in vacuo