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 | — |
Reaction Steps
1.0 g (5.24 mmol) of 2-bromo-4-fluorophenol is initially charged in 4 ml of TFA. Over a period of 20 min, 1.47 g (10.47 mmol) of hexamethylenetetramine are added a little at a time. The mixture is then heated under reflux for 28 h. At RT, 6 ml of water and 3 ml of 50% strength sulfuric acid are added. After 2 h at RT, the reaction mixture is extracted twice with in each case 30 ml of ethyl acetate. The combined organic phases are washed four times with 1N hydrochloric acid and once with water and then dried over magnesium sulfate. The crude product is reacted further without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07732477B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-dc6e313bd581481b9620679b2a7d3673 |
| Source note | uspto-grants-2010_06 |