反应详情

温度

0 °C

To a suspension of ethyl 3-aminoisoquinoline-4-carboxylate (583 mg, 2.70 mmol) in 6.8 mL of H2SO4 5 N cooled to 0° C. was added sodium nitrite (223 mg, 3.24 mmol, dissolved in 1 mL of water). The reaction mixture was stirred at 0° C. for 2.5 h and then NaOH(aq) 1N was added until pH=7. The aqueous phase was extracted twice with DCM and the combined organic phases were dried over MgSO4, filtered and evaporated to give the title compound of Step A which was used without further purification in the next step (583 mg, 99%). MS (ESI) mass calcd. for C12H11NO3, 217.1. m/z found 218.1 [M+H]+.

1. extractionThe aqueous phase was extracted twice with DCM
2. dry with materialthe combined organic phases were dried over MgSO4
3. filtrationfiltered
4. customevaporated