反应详情

温度

115 °C

Ethyl 7-hydroxy-2-(4-methoxyphenyl)pyrazolo[1,5-a]pyrimidine-5-carboxylate (1.26 g; 4.03 mmol) was suspended in phosphoryl chloride (8 mL; 88 mmol) and the mixture was heated to 115° C. for 1 h. The reaction mixture was allowed to cool to room temperature and then carefully quenched into a cold mixture of methylene chloride and saturated sodium bicarbonate. The basic aqueous layer was back extracted once with methylene chloride and the combined organic phases were washed with brine. Concentration afforded a crude solid which was triturated in methanol (15 mL) at 60° C. for 5 min. and then at room temperature for an hour. Filtration afforded 808 mg (60%) of the title compound. LCMS m/z 332.1 (M+H)+, ret. time=2.77 min.

1. temperatureto cool to room temperature
2. customcarefully quenched into a cold mixture of methylene chloride and saturated sodium bicarbonate
3. extractionThe basic aqueous layer was back extracted once with methylene chloride
4. washthe combined organic phases were washed with brine
5. concentrationConcentration
6. customafforded a crude solid which
7. customwas triturated in methanol (15 mL) at 60° C. for 5 min.
8. waitat room temperature for an hour
9. filtrationFiltration