反应详情

To a stirred solution of 1-{3-bromo-4-[(2-pyrazinylmethyl)oxy]phenyl}ethanone (0.2 g) and 1,1-dimethylethyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (0.34 g) in DME (4 ml) was added aqueous sodium carbonate (2M, 0.98 ml). This was degassed with nitrogen for 15 min before adding Tetrakis (37 mg). The reaction was heated under reflux overnight. TLC indicated the reaction had gone to completion and so it was cooled, diluted with water and extracted with ethyl acetate. The combined organics were dried over sodium sulphate and concentrated in vacuo to yield a crude product which was purified by column chromatography, eluting with 0-18% ethyl acetate in hexane. The appropriate fractions were concentrated in vacuo to yield the title compound, 0.093 g, 30% yield.

1. customThis was degassed with nitrogen for 15 min
2. additionbefore adding Tetrakis (37 mg)
3. temperatureThe reaction was heated
4. temperatureunder reflux overnight
5. temperaturewas cooled
6. additiondiluted with water
7. extractionextracted with ethyl acetate
8. dry with materialThe combined organics were dried over sodium sulphate
9. concentrationconcentrated in vacuo
10. customto yield a crude product which
11. customwas purified by column chromatography
12. washeluting with 0-18% ethyl acetate in hexane
13. concentrationThe appropriate fractions were concentrated in vacuo