反应详情

温度

150 °C

A suspension of 66.3 (48 mg, 0.06 mmol), 2-(methylthio)phenylboronic acid (12.5 mg, 0.2 mmol), Na2CO3 (28 mg, 0.24 mmol) in 3:1 DME/H2O (2 mL) was degassed and then added in Pd(PPh3)4 (10 mg). The reaction mixture was heated to 150° C. for 5 min in microwave. The reaction mixture was then partionated between EtOAc and sat. NaCl, the organic layer was collected and dried over (Na2SO4), filtered and concentrated. The crude product of Intermediate 93.1 used as is for the next step. LCMS (4 min gradient) RT=4.87 min, 816.3 (M+H).

1. customwas degassed
2. additionadded in Pd(PPh3)4 (10 mg)
3. customthe organic layer was collected
4. dry with materialdried over (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customLCMS (4 min gradient) RT=4.87 min, 816.3 (M+H)