HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → Methyl 4-bromo-2-(bromomethyl)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Methyl 4-bromo-2-methylbenzoate | HCID 22031226 | — |
| Catalyst | Benzoyl Peroxide | HCID 7187 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | Methyl 4-bromo-2-(bromomethyl)benzoate | HCID 22031079 | 50% |
Reaction Steps
To a solution of 4-bromo-2-methylbenzoic acid methyl ester (1.2 g, 5.2 mmol) in CCl4 (15 mL) was added NBS (0.98 g, 5.5 mmol) and benzoyl peroxide (50 mg, 0.20 mmol). The mixture was heated at reflux for 2 hours under N2 atmosphere. The solvent was evaporated and the residue was purified by chromatography on silica gel (3% ethyl acetate in petroleum) to afford 4-bromo-2-bromomethylbenzoic acid methyl ester (0.80 g, 50%). 1H NMR (CDCl3, 300 MHz) δ 7.84 (d, J=8.4 Hz, 1H), 7.63 (d, J=2.1 Hz, 1H), 7.51 (dd, J=8.4, 2.1 Hz, 1H), 4.90 (s, 2H), 3.94 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324207B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-26e9ab7e0a0445f69975e853a3cf0811 |
| Source note | uspto-grants-2012_12 |