HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-2,4-dimethoxybenzene → HCID 17968171, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-2,4-dimethoxybenzene | HCID 87266 | — |
| Reactant | 4-Bromopyridinium chloride | HCID 88100 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 17968171 | HCID 17968171 | — |
Reaction Steps
The Grignard reagent, prepared from magnesium (5 g) and 1-Bromo-2,4-dimethoxybenzene (38 g) in THF (300 ml), is added at room temperature to 4-Bromo-pyridine hydrochloride salt in THF (10 ml). The mixture is heated under reflux for 2 hours and then evaporated to dryness. The residue is taken up in ethyl acetate and extracted with 1N hydrochloric acid. The aqueous phase is neutralised with 4M sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried with magnesium sulfate, evaporated and the residue is purified by column chromatography on silica gel using n-hexane:AcOEt=1:1 (v/v). MS-APCI+ (M+H)+=216
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07452886B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-5fa6046640ef4ac79636829ba2fcab2e |
| Source note | uspto-grants-2008_11 |