HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Amino-2-chlorophenol → 5-Amino-4-bromo-2-chlorophenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Amino-2-chlorophenol | HCID 80676 | — |
| Reactant | Tetra-n-butylammonium tribromide | HCID 23500184 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Amino-4-bromo-2-chlorophenol | HCID 59377881 | 18% |
Reaction Steps
To a solution of 5-amino-2-chloro-phenol (15.85 g, 110.4 mmol) in dichloromethane (300 ml) and MeOH (150 ml) was added tetrabutylammonium tribromide (58.6 g, 121.4 mmol). The mixture was stirred at room temperature for 20 minutes, and then was partitioned between saturated aqueous Na2SO3 and Et2O. The organic layer was separated, washed with water and brine, dried over MgSO4, filtered and concentrated to dryness under reduced pressure. Purification of the residue by flash chromatography (hex:EtOAc/7:3) gave 5-amino-4-bromo-2-chloro-phenol (4.38 g, 18%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288552B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-b5ff527454fc455cbc4e8654bb11234f |
| Source note | uspto-grants-2012_10 |