HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Bromo-5-fluoro-2-hydroxybenzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Hexamethylenetetramine | HCID 4101 | — |
| Reactant | 2-Bromo-4-fluorophenol | HCID 605472 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 3-Bromo-5-fluoro-2-hydroxybenzaldehyde | HCID 23148955 | 83% |
Reaction Steps
Hexamethylenetetramine (14.7 g, 105 mmol) was slowly added to a solution of 2-bromo-4-fluoro-phenol (10 g, 52.4 mmol) in trifluoroacetic acid (40 ml) at rt and heated to reflux for 18 h. The reaction mixture was cooled to rt and then water (60 ml) and sulfuric acid (30 ml, 50%) were added. The mixture was stirred for 3 h at rt and then extracted twice with ethyl acetate. The combined organic extracts were washed with 1N HCl, water, dried (Na2SO4), filtered and concentrated under reduced pressure to give 9.5 g (83%) of 3-bromo-5-fluoro-2-hydroxy-benzaldehyde.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367676B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-e90f76f50f72495cb9a74e823e9dcb81 |
| Source note | uspto-grants-2013_02 |