Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | Bis(pinacolato)diborane | HCID 2733548 | — |
| Reactant | 6-Methoxy-1,5-naphthyridin-4-yl trifluoromethanesulfonate | HCID 11255265 | — |
| Reactant | [2-(4-Bromo-phenyl)ethyl]-carbamic acid tert-butyl ester | HCID 14221818 | — |
| Catalyst | 1,1`-Bis(diphenylphosphino)ferrocene | HCID 15241612 | — |
| Catalyst | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57938632 | HCID 57938632 | 62% |
Reaction Steps
To a stirred solution of 1,1,1-trifluoromethanesulfonic acid 6-methoxy[1,5]naphthyridin-4-yl ester (1.0 g, 3.24 mmole) in dry dioxane (50 mL) at RT was added bis(pinacolato)diboron (1.07 g, 4.22 mmole), potassium acetate (0.95 g, 9.72 mmole), 1,1-bis(diphenylphosphino)ferrocene (0.09 g, 0.16 mmole) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complexed with dichloromethane (1:1) (0.13 g, 0.16 mmole). The reaction contents were heated to 80° C. for 24 h under nitrogen gas and then 1, 1-bis(diphenylphosphino)ferrocene (0.09 g, 0.16 mmole), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complexed with dichloromethane (1:1) (0.13 g, 0.16 mmole), potassium carbonate (1.34 g, 9.72 mmole) and [2-(4-bromophenyl)ethyl]carbamic acid tert-butyl ester (0.97 g, 3.24 mmole) were added to the reaction pot. After 24 h of vigorous stirring at 80° C., the reaction contents were filtered through a scinter-glass funnel containing a bed of celite (EtOAc). The filtrate was concentrated under vacuum and purified on silica (EtOAc) to afford the title compound (0.76 g, 62%) as a tan solid: LC-MS (ES) m/e 380 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07618959B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-078c1dff49b64af7895598f77119fa38 |
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| Source note | uspto-grants-2009_11 |
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