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温度

0 °C

A mixture of (2-chloro-11-fluoro-5,6-dihydroindolo[1,2-h][1,7]naphthyridin-6-yl)methanol (200 mg, 0.66 mmol) and TEA (200 mg, 1.98 mmol) in THF (8 mL) was stirred at 0° C. and MsCl (114 mg, 0.99 mmol) was added dropwise. The reaction was stirred at RT for 8 h. The reaction was washed with 1N HCl and extracted with DCM, dried with Na2SO4 and concentrated to give (2-chloro-11-fluoro-5,6-dihydroindolo[1,2-h][1,7]naphthyridin-6-yl)methyl methanesulfonate (200 mg, yield: 80%). 1H-NMR (CDCl3, 400 MHz) δ 7.54 (d, J=8.0 Hz, 1H), 7.41 (s, 1H), 7.11˜7.20 (m, 3H), 6.79˜6.83 (m, 1H), 5.03˜5.08 (m, 1H), 4.06˜4.21 (m, 2H), 3.46˜3.52 (m, 1H), 3.24˜3.28 (m, 1H), 2.69 (s, 3H). MS (M+H)+: 381/383.

1. stirringThe reaction was stirred at RT for 8 h
2. washThe reaction was washed with 1N HCl
3. extractionextracted with DCM
4. dry with materialdried with Na2SO4
5. concentrationconcentrated