反应详情

温度

140 °C

200 mg (0.399 mmol) of the compound obtained in example 107 were admixed in a microwavable flask with isopropanol (3 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 140° C. for 2 h. Reaction monitoring showed low conversion. For that reason, N-methylpyrrolidone (1 ml) was added and the mixture was once again heated in a microwave at 140° C. for 2 h and then 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). 21 mg of the title compound were obtained (12% 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. customReaction monitoring
5. temperaturethe mixture was once again heated in a microwave at 140° C. for 2 h
6. temperatureAfter cooling
7. filtrationthe reaction mixture was filtered
8. concentrationconcentrated
9. customthe residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)