反应详情

温度

130 °C

3,4-difluoronitrobenzene (664 mg, 4.18 mmol) was added to a mixture of 7-hydroxy-1,2,4,5-tetrahydro-benzo[d]azepine-3-carboxylic acid tert-butyl ester (WO 02/40471) (1 g, 3.8 mmol) and potassium carbonate (1.3 g, 9.49 mmol) in dimethylformamide (10 ml) and the reaction heated at 130° C. for 3 hours. The reaction was cooled, diluted with ethyl acetate, washed with water and then with a mixture of water:brine (1:1), dried over sodium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography eluting with a mixture of ethyl acetate:pentane (1:10) to afford the title compound. MS (ES+) m/e 303 [M−COOtBu]+.

1. temperatureThe reaction was cooled
2. washwashed with water
3. additionwith a mixture of water:brine (1:1)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by column chromatography
7. washeluting with a mixture of ethyl acetate:pentane (1:10)