反应详情

温度

180 °C

A mixture of 6-(benzenesulphonylmethyl)-3-bromo-2-methoxybenzoic acid (Example 7, 0.1 g), zinc cyanide (0.036 g) and tetrakis-(triphenylphosphine) palladium (0.015 g) in DMF was stirred and heated in the microwave at 180° C. for 10 minutes. After cooling, the mixture was diluted with t-butyl methyl ether, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by preparative HPLC (C18), eluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 35-98% to give 6-(benzenesulphonylmethyl)-3-cyano-2-methoxybenzoic acid (0.02 g) as a white solid.

1. temperatureAfter cooling
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customThe filtrate was evaporated to dryness
5. customthe residue was purified by preparative HPLC (C18)
6. washeluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 35-98%