反应详情

To a solution of the product from Step 1 (31.3 g, 152 mmol) and 4-bromo-3-methoxyaniline (28 g, 139 mmol) in DCM (700 mL) was added PPTS (38.3 g, 152 mmol). The mixture was heated to reflux with stirring for 20 hours and cooled, and the solids removed by filtration and washed with DCM. The filtrate was concentrated and purified on silica (10% to 50% DCM/hexanes) to give the title compound (49 g). LRMS (M+H)+ Calcd.: 376.0; found 376.2.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. temperaturecooled
4. customthe solids removed by filtration
5. washwashed with DCM
6. concentrationThe filtrate was concentrated
7. custompurified on silica (10% to 50% DCM/hexanes)