HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Methyl 3-acetyl-5-bromo-4-hydroxybenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Methyl 3-acetyl-4-hydroxybenzoate | HCID 12332833 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 3-acetyl-5-bromo-4-hydroxybenzoate | HCID 15818980 | 80% |
Reaction Steps
To a stirred solution of methyl 3-acetyl-4-hydroxybenzoate (240 g, 1236 mmol) in DCM (2 L) was added pyridine (0.400 L, 4944 mmol) followed by a dropwise addition of dibromine (0.070 L, 1360 mmol) at 0° C. The reaction mixture was stirred at RT for 2 hrs then cooled to 5° C. and HCl 4N (0.927 L, 3708 mmol) was added dropwise. The organic phase was separated, dried over magnesium sulfate, filtered and concentrated to afford a brown solid which was stirred in ether/petroleum ether (1:1, 1 L) for 1 hr. The solid was collected by filtration and dried to afford methyl 3-acetyl-5-bromo-4-hydroxybenzoate (270 g, 80%) as a beige powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029374B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-78b99fc1897c4e3e94b55135ab6be154 |
| Source note | uspto-grants-2015_05 |