反应详情

100 mg (0.2 mmol) of the compound from Example 43, 20 mg (0.2 mmol) of zinc cyanide and 8 mg (0.007 mmol) of tetrakis(triphenylphosphine)palladium in 2 ml DMF are reacted at 220° C. in a single-mode microwave oven (Emrys Optimizer) for a total of 105 min. After cooling to RT, the reaction mixture is concentrated under reduced pressure and the residue is taken up in formic acid and purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with 0.1% formic acid added to the water). The resulting formate salt is converted into the hydrochloride by addition of 0.5 ml of a 4 N solution of hydrogen chloride in dioxane.

1. concentrationthe reaction mixture is concentrated under reduced pressure
2. custompurified by preparative HPLC (RP18 column
3. additionmobile phase: acetonitrile/water gradient with 0.1% formic acid added to the water)
4. additionThe resulting formate salt is converted into the hydrochloride by addition of 0.5 ml of a 4 N solution of hydrogen chloride in dioxane