反应详情

温度

70 °C

Similar to as described in Example 10, A suspension of 10-bromo-9-fluoro-2-iodo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine (16.0 g, 39.12 mmol, 1.00 equiv)(US2012/245144A1), HMDS (19.3 g, 119.88 mmol, 3.06 equiv) and Pd(dppf)Cl2 CH2Cl2 (1.6 g, 1.95 mmol, 0.05 equiv) in N,N-dimethylformamide (240 mL) was stirred for 2 h at 70° C. under a carbon monoxide atmosphere (1 atm). After cooling to room temperature the reaction was quenched by addition of methanol (5 mL), diluted by ethyl acetate (1 L), washed with water (200×4 mL) and brine (200 mL), dried over sodium sulfate, and concentrated under vacuum. The residue was further purified by FC(Silica and ethyl acetate/petroether 2:1) to give 7.0 g (55%) of the titled compound as a grey solid.

1. temperatureAfter cooling to room temperature the reaction
2. customwas quenched by addition of methanol (5 mL)
3. additiondiluted by ethyl acetate (1 L)
4. washwashed with water (200×4 mL) and brine (200 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customThe residue was further purified by FC(Silica and ethyl acetate/petroether 2:1)