反应详情

温度

80 °C

To a solution of (E)-ethyl 2-(4-(2-(3-(diethoxyphosphoryl)-3,3-difluoropropoxy)ethoxy)-2-methoxybenzylidene)-3-oxobutanoate (1 equiv.) in MeOH (0.20 M) was added guanidine carbonate (1.1 equiv.) and the reaction mixture was heated to 80° C. for 3 h. At this point the reaction mixture was allowed to cool to room temperature and it was then diluted with water and EtOAc. The resulting mixture was transferred to a separatory funnel and washed with EtOAc three times. The combined organic layers were dried over anhydrous Na2SO4 and the volatiles were removed in vacuo. The resulting residue was purified by a COMBIFLASH™ system using a gradient of 0-10% MeOH/DCM to provide the title compound (15%) as a solid.

1. temperatureto cool to room temperature
2. customThe resulting mixture was transferred to a separatory funnel
3. washwashed with EtOAc three times
4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
5. customthe volatiles were removed in vacuo
6. customThe resulting residue was purified by a COMBIFLASH™ system