Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 90286515 | HCID 90286515 | — |
| Reactant | HCID 123702800 | HCID 123702800 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Catalyst | HCID 178526049 | HCID 178526049 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 131735793 | HCID 131735793 | 27.9% |
Reaction Steps
A microwave vial charged with 1-(3-((tert-butyldiphenylsilyl)oxy)bicyclo[3.1.0]hexan-6-yl)-3,3-bis(methylthio)prop-2-en-1-one (2.0 g, 4.1 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-(trifluoro-methoxy)-pyridin-2-amine (1.89 g, 6.23 mmol), ((thiophene-2-carbonyl)oxy)copper (1.58 g, 8.29 mmol), cesium carbonate (2.7 g, 8.3 mmol) and tetra(triphenylphosphine)palladium (0) (957 mg, 0.83 mmol) in 10:1 tetrahydrofuran/water (22 mL) was purged with nitrogen for 3 min. The reaction mixture was sealed and heated by microwave irradiation at 100° C. for 1.5 h. The reaction mixture was concentrated in vacuo, and the resulting residue was purified by flash column chromatography (40% ethyl acetate in petroleum ether) to provide product as a yellow oil (0.70 g, 26% yield). LCMS (ESI) [MH]+=613.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09365583B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-3689c6fc70e841658e98a84eab3ad58e |
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| Source note | uspto-grants-2016_06 |
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