反应详情

Tert-butyl 4-{6-bromo-1-[(2-ethyl-2H-tetrazol-5-yl)methyl]-2,4-dioxo-1,4-dihydrothieno[3,2-d]pyrimidin-3(2H)-yl}piperidine-1-carboxylate (203 mg, B101), 1,3-benzodioxol-5-ylboronic acid (69 mg), dichlorobis(tricyclohexylphosphine)palladium (37 mg) and aqueous cesium carbonate solution (0.375 ml, 2.0 M) are placed in a microwave tube and DME (10 ml) is added. The reaction vessel is sealed and the mixture is subjected to microwave irradiation at 150° C. with stirring for 45 min. After addition of water and extraction with DCM the combined organic layers are washed with saturated aqueous sodium chloride solution and after filtration using a phase separator the organic layer is concentrated. The residue is purified by flash column chromatography [silica gel, elution gradient: cyclohexane/EtOAc, 100/0 to 50/50 to 30/70 (v/v)] to afford the title compound as a solid.

1. customThe reaction vessel is sealed
2. customirradiation at 150° C.
3. washare washed with saturated aqueous sodium chloride solution
4. filtrationafter filtration
5. concentrationis concentrated
6. customThe residue is purified by flash column chromatography [silica gel, elution gradient: cyclohexane/EtOAc, 100/0 to 50/50 to 30/70 (v/v)]