Water → HCID 54266345, compound

Participants

Reaction Steps

A solution of 35.0 mg (0.10 mmol) of Compound J obtained in Reference Example 4 in 3 ml of N,N-dimethylformamide was added dropwise to a mixture of 0.5 ml-N,N-dimethylformamide and 0.5 ml-water containing 3.6 mg (0.02 mmol) of palladium chloride and 2.7 mg (0.02 mmol) of cupric chloride. The reaction mixture was stirred at 50° C. for 2 hours in an oxygen atmosphere, poured into 20 ml of ice water, extracted three times with chloroform. The extracts were washed with water, and with a saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to give 10.4 mg (yield 28%) of 1-(2-oxopropyl)-8-(3-tricyclo[3.3.1.03,7 ]nonyl)-3-propylxanthine (Compound 9) and 9.9 mg (yield 27%) of Compound 11, as a white powder.

Provenance & Evidence