反应详情

温度

130 °C

22-C (63 mg, 0.13 mmol) in TFA (0.65 mL) was treated with triisopropylsilane (0.8 μL, 0.004 mmol). The solution was sealed in a microwave tube and heated to 130° C. for 15 min. The solution was concentrated in vacuo. The residue was purified by reverse phase HPLC to afford a yellow solid (10 mg, 17%). 1H NMR (500 MHz, CD3OD): δ 10.04 (s, 1H), 8.31 (d, J=2.44 Hz, 1H), 7.97 (dd,J=11.2, 2.4 Hz, 1H), 7.14 (d, J=9.27 Hz, 1H), 4.05 (m, 1H), 3.80–3.75 (m, 2H), 3.65–3.47 (m, 2H), 2.52 (m, 1H), 2.22 (m, 1H); LCMS found for C14H15N3O4S (M+H)+: m/z=322.

1. customThe solution was sealed in a microwave tube
2. concentrationThe solution was concentrated in vacuo
3. customThe residue was purified by reverse phase HPLC