反应详情

温度

60 °C

To a suspension of 2-(6-chloro-3-(2-chloroethyl)pyridazin-4-yl)-4-fluoro-1H-indole (60 mg, 0.17 mmol) in DMF (1 mL) was added Cs2CO3 (124 mg, 0.34 mmol), and then the mixture was stirred for 20 minutes at 60° C. After being concentrated in vacuo, the resulting residue was suspended in H2O and extracted with DCM. The combined organic layer was washed with H2O and dried over Na2SO4. After concentration, the residue was purified by prep-TLC (DCM) to give the product of 2-chloro-11-fluoro-5,6-dihydropyridazino[4′,3′:3,4]pyrido[1,2-a]indole (40 mg, yield: 75%). 1H-NMR (CDCl3, 400 MHz) δ 8.40 (s, 1H), 7.63 (s, 1H), 7.47 (d, J=8.22 Hz, 1H), 7.24˜7.33 (m, 1H), 6.87˜6.97 (m, 1H), 4.52 (t, J=6.4 Hz, 2H), 3.53 (t, J=6.4 Hz, 2H). MS (M+H)+: 274/276.

1. concentrationAfter being concentrated in vacuo
2. extractionextracted with DCM
3. washThe combined organic layer was washed with H2O
4. dry with materialdried over Na2SO4
5. concentrationAfter concentration
6. customthe residue was purified by prep-TLC (DCM)