反应详情

温度

105 °C

To 0.52 g of 5-benzyloxymethyl-6-(2-hydroxy-ethyl)pyrazolo[1,5-a]pyrimidin-7(4H)-one were added 4.0 ml of phosphorus oxychloride and 0.55 ml of triethylamine, and the mixture was stirred for 1 hour and 20 minutes in an oil bath heated to 100-110° C. Excess phosphorus oxychloride was distilled off under reduced pressure, and the residue was poured into ice water and extracted with chloroform. After the chloroform layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The thus-obtained crude product was subjected to column chromatography on silica gel (elution solvent: chloroform alone) to obtain 0.37 g (yield: 63.4%) of the intended product.

1. distillationExcess phosphorus oxychloride was distilled off under reduced pressure
2. additionthe residue was poured into ice water
3. extractionextracted with chloroform
4. dry with materialAfter the chloroform layer was dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe thus-obtained crude product
7. washelution solvent