HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → 2-Bromo-1-[3-tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Phenyltrimethylammonium bromide dibromide | HCID 17977687 | — |
| Reactant | 1-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone | HCID 58136808 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | 2-Bromo-1-[3-tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone | HCID 58136782 | 292.5% |
Reaction Steps
1-[3-tert-Butyl-5-(2-methoxyethoxy)phenyl]ethanone (O2.043; 1 g) was dissolved in methanol/THF (25 ml/25 ml), admixed with phenyltrimethylammonium tribromide (882 mg) while stirring and stirred at RT overnight. Then 50 ml of 20% citric acid solution were added and the mixture was stirred for 1 h. Subsequently, DCM (200 ml) was added and the mixture was extracted three times with DCM. Then the combined DCM phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min). 1.31 g of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853206B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-faba81a8a55149ab832e3f163f78ebe1 |
| Source note | uspto-grants-2014_10 |