反应详情

To a solution of crude Compound 2c (10.6 mmol) in methanol (10 mL) was added methyl acetoacetate (10.6 mmol), methyl 3-aminocrotonate (10.6 mmol) and concentrated ammonium hydroxide (1 drop). The reaction mixture was heated at reflux under nitrogen for 4 days. The solvent was removed in vacuo and the residue purified by flash chromatography on silica gel eluted with diethyl ether:hexane (2:1) and trituration with diethyl ether:hexane (1:2) to yield Compound 2d as a pale yellow solid (m.p. 164°-166° C.).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux under nitrogen for 4 days
3. customThe solvent was removed in vacuo
4. customthe residue purified by flash chromatography on silica gel
5. washeluted with diethyl ether:hexane (2:1) and trituration with diethyl ether:hexane (1:2)