Chloroform → 5-Benzyloxymethyl-7-chloro-6-(2-chloroethyl)pyrazolo[1,5-a]pyrimidine

Participants

Reaction Conditions

Reaction Steps

To 0.52 g of 5-benzyloxymethyl-6-(2-hydroxyethyl)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.

Provenance & Evidence