反应详情

温度

130 °C

A mixture of 4-bromo-7-hydroxy-2-phenyl-thiazolo[4,5-c]pyridine-6-carboxylic acid ethyl ester (301.5 mg, 0.80 mmole), methallyltri-n-butyltin (529 μl, 1.60 mmole) and bis(triphenylphosphine)palladium(II) dichloride (56 mg, 0.08 mmole) in dimethylformamide (4 ml) was stirred at 130° C. for 45 min before it was cooled to room temperature, quenched with water, filtered. The filtrate was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and hexanes to give the title compound as a white solid (128 mg). MS: (+) m/z 355.02 (M+1).

1. temperaturewas cooled to room temperature
2. customquenched with water
3. filtrationfiltered
4. customThe filtrate was partitioned between ethyl acetate and water
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and hexanes