HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Acetoxy-5-bromo-6-methylbenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | 3-Bromo-6-hydroxy-2-methylbenzoic acid | HCID 11053451 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-Acetoxy-5-bromo-6-methylbenzoic acid | HCID 11011149 | — |
Reaktionsschritte
A mixture of 1B (6.93 g, 30 mmol), acetic anhydride (3.5 ml, 36 mmol) and pyridine (15 ml) is heated under reflux with stirring for 16 hours. The reaction mixture is diluted with water and ethyl acetate. The organic phase is acidified with dilute hydrochloric acid and washed with water twice. The organic phase is concentrated in vacuo and the residue is purified by flash chromatography (dichloromethane:methanol, 9:1 v/v) yielding the pure product as a yellow oil, 7.4 g, (90.3%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06127570 |
| Quelldatensatz | uspto-grants-2000_10 |
| ORD ID | ord-53b724b373e640f3b1a2566c1fdb3d86 |
| Quellennotiz | uspto-grants-2000_10 |