反应详情

100 mg (0.2 mmol) of the compound from Example 42, 20 mg (0.2 mmol) of zinc cyanide and 8 mg (0.007 mmol) of tetrakis(triphenylphosphine)palladium in 2 ml DMF are reacted for a total of 75 min at 220° C. in a single-mode microwave oven (Emrys Optimizer). 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 by addition of 0.5 ml of a 4 N solution of hydrogen chloride in dioxane into the hydrochloride. The product is washed first with ethyl acetate and then with diethyl ether and dried under reduced pressure.

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 by addition of 0.5 ml of a 4 N solution of hydrogen chloride in dioxane into the hydrochloride
5. washThe product is washed first with ethyl acetate
6. dry with materialwith diethyl ether and dried under reduced pressure