反应详情

温度

160 °C

140 mg (0.473 mmol) 6-(4-tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carbaldehyde are dissolved in 1 ml diethyleneglycoldimethylether. 12 mg (0.028 mmol) 3-diphenylphosphanylpropyl(diphenyl)phosphane and 3.7 mg (0.014 mmol) rhodium(III)-chloride trihydrate are added. The reaction mixture is stirred for 42 hours at 160° C. The mixture is cooled to room temperature and partitioned between dichloromethane and water. The organic phase is dried over sodium sulfate and evaporated. The residue is chromatographed on a silica gel column with cyclohexane/ethyl acetate as eluent to give 6-(4-tert-butyl-phenyl)-5H-pyrazolo[1,5-a]pyrazin-4-one (“A15”) as colourless crystals; HPLC/MS: 1.88 (C), [M+H] 268.

1. temperatureThe mixture is cooled to room temperature
2. custompartitioned between dichloromethane and water
3. dry with materialThe organic phase is dried over sodium sulfate
4. customevaporated
5. customThe residue is chromatographed on a silica gel column with cyclohexane/ethyl acetate as eluent