反应详情

2 g (5.98 mmol) of ethyl 7-(benzyloxy)-2,5-dimethylpyrazolo[1,5-a]pyridine-3-carboxylate from Example 7A were initially charged in 80 ml of ethanol under argon, and 636 mg (0.59 mmol, 10%) of palladium on activated carbon and 18 ml (179.42 mmol) of cyclohexene were added. The reaction mixture was stirred under reflux for 2.5 hours. Then the reaction mixture was filtered through kieselguhr and washed with ethanol, and the filtrate was concentrated. The residue was taken up in DMSO and acetonitrile and purified by means of preparative HPLC (RP 18 column, eluent:acetonitrile/water gradient with addition of 0.1% TFA). The product fractions were combined, concentrated and lyophilized. 1.2 g of the target compound were obtained (86% of theory).

1. temperatureunder reflux for 2.5 hours
2. filtrationThen the reaction mixture was filtered through kieselguhr
3. washwashed with ethanol
4. concentrationthe filtrate was concentrated
5. customacetonitrile and purified by means of preparative HPLC (RP 18 column, eluent:acetonitrile/water gradient with addition of 0.1% TFA)
6. concentrationconcentrated