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 1N 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 1N 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)