Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | 5-bromo-1-(2-hydroxyethyl)pyridin-2(1H)-one | HCID 43419433 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1016530-65-6 | HCID 24689280 | — |
Reaction Steps
To a solution of 5-bromo-1-(2-hydroxyethyl)pyridin-2(1 H)-one (460 mg, 2110 μmol) in CH2Cl2 (5 mL) at 0° C. under nitrogen was added phosphorous tribromide (595 μL, 6329 μmol). A precipitate formed at 0° C. The reaction mixture was heated at 40° C. for 3 days. The mixture was partitioned between CH2Cl2 and 5% NaHCO3 (vigorous gas evolution). The aqueous was extracted with CH2Cl2 (2×10 mL). The combined organics were dried over MgSO4, and concentrated to a white solid. MS (ESI pos. ion) m/z (MH+): 279/281/283. Calc'd exact mass for C7H7Br2NO: 278.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08314087B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-b7108dabcc054546a4fc258ceaa0349d |
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| Source note | uspto-grants-2012_11 |
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