反应详情

1-Bromo-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid methyl ester (0.2 g), tetrakis(triphenylphosphine)palladium (60 mg), methyl boroxine (65 mg), and potassium carbonate in 1,4-dioxane (4 ml) were heated in a microwave reactor (sealed tube) for 10 min at 140° C. After cooling reaction mixture was concentrated and partitioned between 1 N hydrochloric acid and ethyl acetate. Organic layer dried over magnesium sulfate and filtered. Filtrate concentrated and separated by silica gel chromatography (eluting with 2% ethyl acetate in methylene chloride) to give the title compound (47 mg). MS-(+)-ion M+1=326.1.

1. custom(sealed tube) for 10 min at 140° C
2. temperatureAfter cooling
3. customreaction mixture
4. concentrationwas concentrated
5. custompartitioned between 1 N hydrochloric acid and ethyl acetate
6. dry with materialOrganic layer dried over magnesium sulfate
7. filtrationfiltered
8. concentrationFiltrate concentrated
9. customseparated by silica gel chromatography (eluting with 2% ethyl acetate in methylene chloride)