Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | HCID 178516492 | HCID 178516492 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 59186792 | HCID 59186792 | — |
Reaction Steps
2-Pyridin-4-yl-pyrimidin-4-ol (200 mg, 1.16 mmol) was suspended in DCE (10 mL) then POBr3 (497 mg, 1.73 mmol) was added in one portion. The reaction mixture was heated to 95° C. (bath) for 18 h then cooled to 20° C. H2O (30 mL) and CH2Cl2 (30 mL) were added, then the biphasic mixture was stirred vigorously for 30 min. The layers were separated and the aqueous phase was extracted with CH2Cl2 (3×30 mL). The combined organics were evaporated to dryness to afford the title compound: m/z (ES+)=236, 238 (1:1) [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08173807B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-b64558471e924489ae7bc84849027077 |
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| Source note | uspto-grants-2012_05 |
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