HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Ethyl-5-methoxyphenol → 4-Bromo-5-methoxy-2-ethyl-phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Ethyl-5-methoxyphenol | HCID 12529751 | — |
| Reactant | Tetra-n-butylammonium tribromide | HCID 23500184 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-Bromo-5-methoxy-2-ethyl-phenol | HCID 58764076 | 104.1% |
Reaction Steps
A solution of tetrabutyl ammonium tribromide (38.10 g, 79 mmol) in CHCl3 (100 mL) was added to a stirred solution of 5-methoxy-2-ethyl-phenol (12.0 g, 79 mmol) dissolved in CHCl3 (90 mL). The reaction mixture was stirred for 4 hrs and then quenched with 5% solution of sodium thiosulfate (90 mL). The biphasic mixture was stirred for 30 mins and then the layers were separated. The organic layer was washed with 1 N HCl, brine, dried over Na2SO4 and concentrated to a red oil. Purification by flash column chromatography (0% to 60% EtOAc in hexanes) gave the product as an oil (19 g). LCMS: APCI−VE=230 M/E.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268835B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-3363795589d047c5b98f961d846b74f4 |
| Source note | uspto-grants-2012_09 |