反应详情

PPTS (38.3 g, 152 mmol) was added 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). The mixture was heated to reflux and stirred for 20 h. The mixture was cooled, and the solids were removed by filtration and washed with DCM. The filtrate was concentrated and purified on silica gel (gradient elution 10% to 50% DCM in hexanes) to give the title compound (49 g, 94% yield). LRMS (M+H)+ Calcd.: 376.0; found 376.2.

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