HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19387210, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 19387264 | HCID 19387264 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 19387210 | HCID 19387210 | 236.2% |
Reaction Steps
6-bromo-2,2-dimethyl-3-hydroxymethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran (9.0 g, 0.0248 mol) was suspended in toluene (150 ml). Phosphorus tribromide (0.94 ml, 2.69 g, 0.0099 mol) was added and the mixture heated at reflux for two hours. The cooled solution was treated with water and ethyl acetate, the organic phase separated and washed three times with aqueous sodium chloride solution, and then dried and evaporated under reduced pressure. The residue was triturated with pentane and dried to afford 9.94 g of 6-bromo-2,2-dimethyl-3-bromomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran, m.p. 175° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05447943 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-a47a4c9858564a7681f56d9ac4f5ad6b |
| Source note | uspto-grants-1995_09 |