反应详情

19 mg (0.29 mmol) of copper powder were added to 3.57 g (81% purity, 5.87 mmol) of the compound from Example 24A in 15 ml of pyridine and 8 ml of ethanol. The reaction mixture was heated under reflux for 5 h and then the copper was filtered off through kieselguhr. The filtrate was concentrated, the residue was stirred with diethyl ether/dichloromethane, and the precipitated solid was filtered off. The filtrate was concentrated and purified by preparative HPLC (acetonitrile/water gradient). 1.24 g (46% of theory) of the title compound were obtained.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 5 h
3. filtrationthe copper was filtered off through kieselguhr
4. concentrationThe filtrate was concentrated
5. filtrationthe precipitated solid was filtered off
6. concentrationThe filtrate was concentrated
7. custompurified by preparative HPLC (acetonitrile/water gradient)