HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-o-xylene → HCID 18696680, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-o-xylene | HCID 32886 | — |
| Reactant | Dimethylmalonyl Dichloride | HCID 4523180 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18696680 | HCID 18696680 | 83% |
Reaction Steps
To a mixture of 35.5 ml of 4-chloro-o-xylene and 29.84 g of dimethylmalonyl chloride in 150 ml of dry dichloromethane was added slowly 34.7 g of AlCl3 under the current of nitrogen gas at -10° C. The reaction mixture was stirred at room temperature for 2 hours, quenched with 200 g of ice, and separated the organic layer. The aqueous layer was extracted with dichloromethane. The combined organic layer was dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by silica-gel column chromatography to afford 34.99 g of the title compound as yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06096930 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-b3f21784b0d7430d8b970bda37694360 |
| Source note | uspto-grants-2000_08 |