Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86701006 | HCID 86701006 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86701053 | HCID 86701053 | 83% |
Reaction Steps
Pyridine (2.8 mL, 36.0 mmol was added to a solution of tert-butyl 4-(2-((2S,5R)-6-(benzyloxy)-7-oxo-1,6-diaza-bicyclo[3.2.1]octane-2-carbonyl)hydrazine-carbonyl)piperazine-1-carboxylate (903 mg, 1.8 mmol) in DCM (200 mL). (CF3SO2)2O (2.8 ml, 9.0 mmol) was then added slowly at −10° C. The reaction mixture was stirred at rt for 3 hrs. Saturated NaHCO3 was added at −10° C. very slowly. The combined organic layer was separated and the aqueous layer was exacted with EtOAc (3×). The combined organic layer was dried over Na2SO4, and concentrated. The crude product was purified by silica gel column chromatography (2:1 EtOAc/hexanes) to give tert-butyl 4-(5-((2S,5R)-6-(benzyloxy)-7-oxo-1,6-diaza-bicyclo[3.2.1]octan-2-yl)-1,3,4-oxadiazol-2-yl)piperazine-1-carboxylate (723 mg, 83%) as a slight yellow solid. ESI-MS (EI+, m/z): 485.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08969570B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-d24939952921477d84b08416fdeb80b4 |
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| Source note | uspto-grants-2015_03 |
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