HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 66790679, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| Reactant | Benzoyl chloride, 3,4-dichloro- | HCID 76403 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 66790679 | HCID 66790679 | 63% |
Reaction Steps
A mixture comprising 10.0 g of 3,4-dichlorobenzoyl chloride, 9.31 g of ethyl 2-bromoisobutyrate and 90 ml of anhydrous diethyl ether, was dropwise added to 3.12 g of zinc in a nitrogen atmosphere, followed by a reaction for 15 hours under reflux. The reaction mixture was filtered through celite, and the filtrate was washed with 20% sulfuric acid and then with water. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate/n-hexane=1/19) to obtain 8.7 g of oily ethyl 2-(3′,4′-dichlorobenzoyl)isobutyrate. The NMR spectrum data of this product is as follows.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08039420B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-9e0883f571f34aaca82db3250974e00e |
| Source note | uspto-grants-2011_10 |