HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → 1372891-51-4
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 68277844 | HCID 68277844 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1372891-51-4 | HCID 86691606 | 104.6% |
Reaction Steps
Intermediate 6 ((3-fluoro-4-methyl-2-pyridinyl)methanol, 246 mg, 1.743 mmol) was dissolved in 10 mL of anhydrous THF. Phosphorous tribromide (ALDRICH, 519 mg, 1.917 mmol) was added. Reaction mixture was stirred at room temperature overnight. Solvent was evaporated and residue was partitioned between Et2O and NaHCO3 (aqueous saturated solution). Organic layer was dried over MgSO4 (anh), filtered and concentrated to give the title compound (372 mg, quantitative yield). 1H NMR (300 MHz, DMSO-d6) ppm: 8.23-8.24 (m, 1H), 7.34-7.37 (m, 1H), 4.66 (s, 2H), 2.28 (s, 3H). [ES+MS] m/z 204 (M).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09334265B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-d849e95669d446418060b9ac1007d34e |
| Source note | uspto-grants-2016_05 |