反应详情

温度

80 °C

A mixture of 3-cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-ol (E3) (1.5 g), dimethyl 6-chloro-2,3-pyridinedicarboxylate (1.58 g; Kenji Niiyama et al. Bioorg. Med. Chem. Lett. 12, 21, 2002, 3041-3054) and cesium carbonate (4.4 g) in dry DMF (30 ml) was heated at 80° C. for 3 h. The cooled mixture was partitioned between water (20 ml) and ethyl acetate (3×100 ml), the combined organic extracts were washed with brine (2×100 ml) and dried (Na2SO4). The solvent was evaporated to give an oil which was purified by column chromatography eluting with a mixture of 0.880 ammonia:methanol:dichloromethane (0.5:4.5:95) to afford the title compound (E231); MS (ES+) m/e 411 [M+H]+.

1. customThe cooled mixture was partitioned between water (20 ml) and ethyl acetate (3×100 ml)
2. washthe combined organic extracts were washed with brine (2×100 ml)
3. dry with materialdried (Na2SO4)
4. customThe solvent was evaporated
5. customto give an oil which
6. customwas purified by column chromatography
7. washeluting with a mixture of 0.880 ammonia:methanol:dichloromethane (0.5:4.5:95)