反应详情

温度

80 °C

A mixture of 1,3-dimethyl-2,4-dioxo-6-((2-(trimethylsilyl)ethoxy)methyl)-2,3,4,6-tetrahydro-1H-pyrrolo[3,4-d]pyrimidin-5-ylboronic acid (Intermediate Ga Step 2) (7.31 g, 20.7 mmol), 1-bromo-3-fluorobenzene (2.10 mL, 18.8 mmol), Pd-118 (245 mg, 0.38 mmol), and barium hydroxide (6.44 g, 37.6 mmol) in n-butyl acetate (64 mL) was heated to 80° C. Water (4.06 mL, 226.0 mmol) was added and the mixture was stirred vigorously at 80° C. for 30 minutes. The reaction mixture was cooled to room temperature diluted with 1M HCl(aq) (100 mL) and was extracted with DCM (3×100 mL). The combined organic layers were washed with saturated brine (1×100 mL), dried over magnesium sulfate and the evaporated under vacuum. The residue was recrystallised from methanol to afford the title compound.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionwas extracted with DCM (3×100 mL)
3. washThe combined organic layers were washed with saturated brine (1×100 mL)
4. dry with materialdried over magnesium sulfate
5. customthe evaporated under vacuum
6. customThe residue was recrystallised from methanol