反应详情

温度

50 °C

A mixture of 5-(1-azetidin-3-yl-1H-pyrazol-4-yl)-3-[1-(2,6-dichloro-3-fluorophenyl)-ethyl]-1H-pyrrolo[2,3-b]pyridine (6.0 mg, 0.014 mmol) and ethyl formate (2 mL) was heated to 50° C. overnight in a sealed tube. The solution was concentrated in vacuo, redissolved in MeOH and purified via HPLC. The fractions containing the pure product were concentrated in vacuo to afford the title compound as a white solid. 1H NMR (400 MHz, CD3OD): δ=1.89 (d, J=7.3 Hz, 3 H), 4.37 (ddd, J=6.2, 5.1, 4.9 Hz, 1 H), 4.46-4.54 (m, 1 H), 4.60 (dd, J=9.2, 5.4 Hz, 1 H), 4.71 (t, J=8.6 Hz, 1 H), 5.30 (q, J=7.3 Hz, 1 H), 5.38 (tt, J=8.2, 5.5 Hz, 1 H), 7.16-7.23 (m, 1 H), 7.38 (d, J=1.3 Hz, 1 H), 7.39-7.57 (m, 2 H), 7.72 (s, 1 H), 7.95 (s, 1 H), 8.07 (s, 1 H), 8.33 (d, J=1.8 Hz, 1 H). MS (ES+): m/z 458.06 (100) [MH+]. HPLC: tR=3.22 min (ZQ3, polar—5 min).

1. concentrationThe solution was concentrated in vacuo
2. dissolutionredissolved in MeOH
3. custompurified via HPLC
4. additionThe fractions containing the pure product
5. concentrationwere concentrated in vacuo