反应详情

A mixture of 1-bromo-7-(4-fluoro-phenoxy)-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (434 mg, 1 mmol), Pd(PPh3)4 (116 mg, 0.1 mmol), trimethylboroxine (140 μl, 1 mmol), K2CO3 (414 mg, 3 mmol), and 1,4-dioxane (8 ml) was refluxed with stirring for 2 h. Subsequently, the mixture was concentrated in vacuo. To the residue was added water (10 ml). The mixture was acidified by the addition of aqueous 6N HCl and then extracted with EtOAc (40 ml). The organic phase was dried over MgSO4 and evaporated in vacuo. Purification of the residue by flash column chromatography on silica gel using hexanes:EtOAc=94:6 as the eluent gave the title compound as white solid (229 mg); MS-(+)-ion: M+1=370.1.

1. temperaturewas refluxed
2. concentrationSubsequently, the mixture was concentrated in vacuo
3. additionTo the residue was added water (10 ml)
4. additionThe mixture was acidified by the addition of aqueous 6N HCl
5. extractionextracted with EtOAc (40 ml)
6. dry with materialThe organic phase was dried over MgSO4
7. customevaporated in vacuo
8. customPurification of the residue by flash column chromatography on silica gel