HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → Methyl 2-(4-fluorophenethyl)-5-bromomethylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Methyl 2-(4-fluorophenethyl)-5-hydroxymethylbenzoate | HCID 18474618 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 2-(4-fluorophenethyl)-5-bromomethylbenzoate | HCID 18474623 | 58.3% |
Reaction Steps
A mixture of methyl 2-(4-fluorophenethyl)-5-hydroxymethylbenzoate (13.10 g., 45.43 mmol), carbon tetrabromide (18.08 g, 54.52 mmol) and triphenylphosphine (14.30 g, 54.52 mmol) in dichloromethane (400 ml) was stirred at ambient temperature for 4 hours. More carbon tetrabromide (7.54 g, 23.00 mmol) and triphenylphosphine (5.96 g, 23.00 mmol) in dichloromethane (50 ml) were added and then stirred for a further 2 hours. The reaction was applied directly to a silica flash column and eluted with iso-hexane/ethyl acetate (92.5:7.5) to give as a clear gum methyl 2-(4-fluorophenethyl)-5-bromomethylbenzoate (9.30 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06414145B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-d5173071816749ddb1552c8d6cc1fe5f |
| Source note | uspto-grants-2002_07 |