反应详情

温度

90 °C

To a solution of 0.72 g of 8-[(6-bromopyridin-2-yl)-(tert-butyldimethylsiloxy)methyl]-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine in N,N-dimethylformamide (8 ml) were added 0.17 ml of ethyl acrylate, 0.22 ml of triethylamine, 12 mg of palladium (II) acetate and 33 mg of triphenylphosphine and the resulting mixture was heated to 90° C. for 30 hours. Then the reaction mixture was brought back to room temperature and distributed into water and ethyl acetate. The organic layer was extracted, washed successively with water and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and filtered. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (diluted with dichloromethane/ethyl acetate) to thereby give 540 mg of the title compound as a yellow oily substance.

1. customwas brought back to room temperature
2. extractionThe organic layer was extracted
3. washwashed successively with water
4. dry with materiala saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. distillationAfter distilling off the solvent under reduced pressure
7. customthe residue was purified by silica gel column chromatography (diluted with dichloromethane/ethyl acetate)