Phosphorus oxychloride → HCID 86636111, compound

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence