反应详情

温度

80 °C

A mixture of 4-(6-methoxy-4-oxo-4,5-dihydro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (1 mmol), phosphorus oxychloride (2 mmol) and dimethylformamide (5 drops) is heated at 80° C. for 6 h. The mixture is allowed to cool, the solvent is evaporated and the residue is poured into ice-water. The mixture is extracted three times with ethyl acetate. The combined ethyl acetate extracts are washed with brine, dried (magnesium sulfate), filtered, and evaporated to give crude 4-(4-chloro-6-methoxy-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester.

1. temperatureto cool
2. customthe solvent is evaporated
3. additionthe residue is poured into ice-water
4. extractionThe mixture is extracted three times with ethyl acetate
5. washThe combined ethyl acetate extracts are washed with brine
6. dry with materialdried (magnesium sulfate)
7. filtrationfiltered
8. customevaporated