Synthesis of 2- 3-methoxyphenyl)-N-phthalazin-1-yl-acetamide
Phthalazin-1-ylamine (57 mg; 0.39 mmol) was suspended in 1 ,2-dichloro-ethane (4 mL) under argon. N-ethyldiisopropylamine (0.141 mL; 0.83 mmol) was added followed by the dropwise addition of (3-methoxyphenyl)-acetyl chloride (0.123 ml; 0.79 mmol) via a syringe. During the addition the temperature increased from 20 °C to 35 °C. After one minute a clear light brown solution was obtained. The reaction was stirred for 18 h at room temperature. The solvent was removed under vacuum. The residue was purified by chromatography (column: 40 g RP18 silica gel; combiflash companion); yield: 6 mg (5 %), colourless solid (purity: 100 %, Rt: 2.94 min);
1H NMR (400 MHz, DMSO-d6) δ [ppm] 10.96 (s, 1H), 9.59 (s, 1 H), 8.19 (d, J = 8.0 Hz, 1 H), 8.08 - 7.79 (m, 3H), 7.29 (t, J = 7.9 Hz, 1 H), 7.10 - 6.74 (m, 3H), 3.86 (s, 2H), 3.77 (s, 3H).
WO2014206524
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