Reaktion #971092
ord-0e251fb25a3340f28cf1e0ec89309680
Reaktionsgleichung
Edukte
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1SonstigeConsumption of starting material
Vorschrift
The product from Example 36e (0.040 g, 0.24 mmol) was reacted with the product from Example 22b as a 1.5M solution in ethanol (0.162 mL, 0.24 mmol) for 17.5 h at 100° C. following the procedure from Example 7g. Consumption of starting material required a second addition of the product from Example 36e (0.027 g, 0.16 mmol) and continued heating at 100° C. (24 h) giving the crude title compound which was purified by HPLC with TFA providing the product as a trifluoroacetic acid salt (0.038 g, 27%). 1H NMR (300 MHz, DMSO-d6) δ ppm: 2.02 (s, 3 H) 2.36 (s, 3 H) 7.12-7.37 (m, 5 H) 7.38-7.53 (m, 3 H) 7.73-7.92 (m, J=8.64, 4.60 Hz, 2 H) 8.94 (d, J=8.46 Hz, 1 H) 9.18 (d, J=4.04 Hz, 1 H) 9.99 (s, 1 H); MS (ESI+) m/z 401.3 (M+H)+; (ESI−) m/z 399.0 (M−H)−.