反应详情

温度

180 °C

200 mg (0.399 mmol) of the compound obtained in example 107 were admixed in a microwavable flask with methanol (3 ml), N-methylpyrrolidone (1 ml), 260 mg (0.798 mmol) of cesium carbonate, 8 mg (0.04 mmol) of copper(I) iodide and 19 mg (0.08 mmol) of 3,4,7,8-tetramethyl-1,10-phenanthroline. The flask was purged with argon while being treated with ultrasound for 5 min, and then closed with an appropriate septum. Then it was heated in a microwave at 180° C. for 8 h. After cooling, the reaction mixture was filtered and concentrated, and the residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). 17 mg of the title compound were obtained (10% of theory).

1. customThe flask was purged with argon
2. additionwhile being treated with ultrasound for 5 min
3. customclosed with an appropriate septum
4. temperatureAfter cooling
5. filtrationthe reaction mixture was filtered
6. concentrationconcentrated
7. customthe residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)