Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | HCID 70558151 | HCID 70558151 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86725376 | HCID 86725376 | — |
Reaction Steps
A mixture of the product of Example 15A (5.12 g, 13.2 mmol), tert-butyl piperazine-1-carboxylate (2.95 g, 15.8 mmol), palladium diacetate (149 mg, 0.66 mmol), (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthalene (616 mg, 0.99 mmol) and cesium carbonate (8.61 g, 26.4 mmol) in toluene (100 mL) was heated at 100° C. under nitrogen for 16 hours. After cooling, the mixture was filtered and the filtrate was concentrated. The residue was purified by flash chromatography on silica gel (200-300 mesh) eluting with 5/1 petroleum ether/ethyl acetate to give the title compound. MS: 494 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09212192B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-1b6ad56bcce14ddcacc2c36e90f26e75 |
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| Source note | uspto-grants-2015_12 |
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