HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Ethyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 2-(4-(4-Chlorobutanoyl)phenyl)-2-methylpropanoic acid | HCID 10923567 | — |
| Product | Ethyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate | HCID 11231785 | 97% |
Reaction Steps
Add anhydrous hydrogen chloride gas (18.0 g) to anhydrous ethanol DB (210 g) by purging the solution. Add this hot solution (60° C.) to a solution of 2-[4-(4-chloro-butyryl)-phenyl]-2-methyl-propionic acid (31 g, 115.6 mmol) and reflux under a nitrogen atmosphere for 2.5 hours. Evaporate the solvent in vacuo, dissolve the residue in methylene chloride (150 mL) and wash with water (2×100 mL). Dry (MgSO4), filter through silica gel, washing the gel with methylene chloride (250 mL). Combine the organic washings and evaporate the solvent in vacuo to give the title compound as a colorless oil (33.3 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06566526B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-97e4b51c165d455f95c9d3909ed95052 |
| Source note | uspto-grants-2003_05 |