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 (step 2) (2.0 g, 5.7 mmol), 3-bromobenzonitrile (937 mg, 5.2 mmol), Pd-118 (168 mg, 0.26 mmol) and potassium carbonate (1.42 g, 10.3 mmol) in n-butyl acetate (40 mL) was heated to 80° C., then water (2.23 mL, 124.0 mmol) was added and the mixture was heated at 80° C. for 90 minutes. The reaction mixture was diluted with water (100 mL), the layers were separated as much as possible, and the aqueous phase (and residual organic portion) was extracted with DCM (1×100 mL, 2×50 mL). The combined organic extracts were washed with brine (1×100 mL), dried with magnesium sulfate and the solvent was removed under vacuum. The resulting residue was re-crystallised from methanol and dried under vacuum at 50° C. to afford the title compound;

1. temperaturethe mixture was heated at 80° C. for 90 minutes
2. customthe layers were separated as much as possible, and the aqueous phase (and residual organic portion)
3. extractionwas extracted with DCM (1×100 mL, 2×50 mL)
4. washThe combined organic extracts were washed with brine (1×100 mL)
5. dry with materialdried with magnesium sulfate
6. customthe solvent was removed under vacuum
7. customThe resulting residue was re-crystallised from methanol
8. customdried under vacuum at 50° C.