HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22114930, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | HCID 54409558 | HCID 54409558 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22114930 | HCID 22114930 | 57% |
Reaction Steps
6 ml of 85% strength phosphoric acid and 6 ml of H2O were added dropwise to 2.6 g (10 mmol) of methyl 2,4-dichloro-3-(2-methoxyethen-1-yl)benzoate in 80 ml of dioxane. The mixture was heated under reflux for 12 hours and then stirred at room temperature for 12 hours. The solvent was removed and the residue was taken up in ethyl acetate, washed with 10% strength sodium bicarbonate solution, dried and concentrated. The residue was chromatographed over silica gel (eluent: cyclohexane:ethyl acetate=9:1). 1.4 g (57% of theory) of methyl 2,4-dichloro-3-(2-oxoeth-1-yl)benzoate were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06165944 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-ef61a9efae514e619f36102cdf8ca504 |
| Source note | uspto-grants-2000_12 |