反应详情

温度

160 °C

To a solution of compound 3 (316 mg, 1.7 mmol) and compound 5 (507 mg, 2.55 mmol) in DMF (25 mL) was added ZnCl2 (232 mg, 1.7 mmol). The reaction mixture was stirred at 160° C. overnight. Then the reaction mixture was diluted with aqueous NaOH (10%) and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure, the residue was purified by column chromatography (hexane: EtOAc=20:1) to give 13 mg of the target product (2.1%). MS [M++1]=368, LC-MS: tR=1.909 min

1. extractionextracted with EtOAc
2. dry with materialThe organic layer was dried over anhydrous Na2SO4
3. customthe solvent was removed under reduced pressure
4. customthe residue was purified by column chromatography (hexane: EtOAc=20:1)