HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → Ethyl 2-bromomethyl-6-methoxybenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2-Methoxy-6-methyl-benzoic acid ethyl ester | HCID 591060 | — |
| Catalyst | Azobisisobutyronitrile | HCID 6547 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | Ethyl 2-bromomethyl-6-methoxybenzoate | HCID 10038926 | 85% |
Reaction Steps
2-Methoxy-6-methylbenzoic acid ethyl ester (500 mg, 2.67 mmol), N-bromosuccinimide (483.8 mg, 2.72 mmol) and 2,2′-azobis(2-methyl-propionitrile) (30.2 mg, 0.123 mmol) in carbon tetrachloride (10 ml) were heated to reflux. After 18 hours, the reaction mixture was evaporated to dryness in vacuo. The residue was dissolved in dichloromethane (100 ml) and washed with water (2×50 ml). The organic layer was dried (MgSO4), filtered and the solvent evaporated in vacuo. The residue (702 mg) was purified by column chromatography using a mixture of hexanes/dichloromethane (1:1) as eluent, which afforded 573 mg (85%) of 6-bromomethyl-2-methoxy-benzoic acid ethyl ester as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115624B1 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-7c8ea013f76149cc82bee8fdc9af5c3b |
| Source note | uspto-grants-2006_10 |