反应详情

温度

90 °C

A RBF charged with xantphos (9.97 g, 17.23 mmol), pd2(dba)3 (5.26 g, 5.74 mmol), 4-bromo-1-iodo-2-methoxybenzene (74.9 g, 239 mmol), (E)-ethyl 3-(2-amino-5-(benzylthio)phenyl)acrylate (60.000 g, 191 mmol), cesium carbonate (100 g, 306 mmol), and 400 ml cylopentyl-methylether was heated to 90° C. overnight. The reaction mixture was then poured into water and extracted with DCM. The organics were dried over MgSO4 and concentrated. The crude residue was triturated with IPA leaving a yellow solid that was collected and dried yielding (E)-ethyl 3-(5-(benzylthio)-2-((4-bromo-2-methoxyphenyl)amino)phenyl)acrylate (86.95 g, 174 mmol, 91% yield). m/z (ESI) 500.1 (M+H)+.

1. extractionextracted with DCM
2. dry with materialThe organics were dried over MgSO4
3. concentrationconcentrated
4. customThe crude residue was triturated with IPA leaving a yellow solid
5. customthat was collected
6. customdried