反应详情

温度

100 °C

A mixture of 2-cyclopropylpyrazolo[1,5-a]pyrimidin-7-ol (0.400 g, 2.28 mmol) and phosphorous oxychloride (4.26 ml, 45.7 mmol) in a resealable tube was heated to 100° C. After 4 hrs the solution was cooled to RT and slowly poured onto ice. The mixture was made basic using 2 N NaOH and saturated NaHCO3 and extracted with EtOAc. The combined organic fractions were washed with brine and dried with sodium sulfate. The organic phase solution was passed over a plug of silica gel and concentrated in vacuo to afford 7-chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidine as a brown oil that was advanced without further purification. MS: Found M+H+=194.1.

1. temperatureAfter 4 hrs the solution was cooled to RT
2. additionslowly poured onto ice
3. extractionextracted with EtOAc
4. washThe combined organic fractions were washed with brine
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated in vacuo