HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-(Bromomethyl)-3,5-difluoropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | (3,5-Difluoropyridin-4-yl)methanol | HCID 66815317 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-(Bromomethyl)-3,5-difluoropyridine | HCID 66815097 | 83% |
Reaction Steps
To a solution of (3,5-difluoropyridin-4-yl)methanol (3.5 mmol) in anhydrous chloroform (15 mL) was added dropwise a solution of phosphorus tribromide (330 μL, 3.5 mmol) in anhydrous chloroform (5 mL) at 0° C. The mixture was stirred for 6 hours at room temperature. Water was added, and the reaction was extracted 3 times with dichloromethane. The combined organic phases were washed with brine and dried over magnesium sulfate. After evaporation of the solvent, 4-(bromomethyl)-3,5-difluoropyridine was obtained as pale yellow solid (600 mg, 83% yield for 2 steps) and used in the next step without purification; 1H NMR (400 MHz, MeOd4): δ 4.59 (s, 2H), 8.42 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040538B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-802b32d49c4a4d679b677987b93b47a5 |
| Source note | uspto-grants-2015_05 |