反应详情

To 6-bromo-1,3-bis-(tert-butyl-dimethyl-silanyloxy)-isoquinoline (1.76 g, 3.75 mmole) is added tetrakis(triphenylphosphine)palladium (110 mg, 0.095 mmole) and 2M cyclopentyl magnesium bromide in ether (3.0 mL, 6.0 mmole). This mixture is heated using a microwave reactor at 75° C. for 600 sec. The mixture is cooled to room temperature, transferred to a flask with THF and water, then 2M hydrochloric acid (20 mL) is added and stirred for 4 hours at room temperature. The organic solvents were removed in vacuo, the mixture extracted with ethyl acetate, the organic layer dried over sodium sulfate filtered, evaporated and chromatographed with hexanes-ethyl acetate on silica gel to give a white solid, 268 mg (31%) MS (ESI): m/z 230.2 (M+H).

1. temperatureThis mixture is heated
2. customat 75° C.
3. customfor 600 sec
4. customThe organic solvents were removed in vacuo
5. extractionthe mixture extracted with ethyl acetate
6. dry with materialthe organic layer dried over sodium sulfate
7. filtrationfiltered
8. customevaporated
9. customchromatographed with hexanes-ethyl acetate on silica gel
10. customto give a white solid, 268 mg (31%)