HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → HCID 11152275, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | HCID 11148398 | HCID 11148398 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 11152275 | HCID 11152275 | 60.3% |
Reaction Steps
To a solution of 8.03 g (39.3 mmol) of 5-ethoxycarbonyl-2-methylimidazo[1,2-a]pyridine and 14.41 g (118 mmol) of 4-dimethylaminopyridine in 80 ml of chloroform was added dropwise 21.45 g (118 mmol) of trichloroacetyl chloride. The mixture was heated for 15 hours under reflux. After cooling, the reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, drid over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent:ethyl acetate/n-hexane=2:1) to give 8.29 g of the desired compound (60.3%, pale yellow solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06251905B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-d0df75025d72427ebc55bda974b9211f |
| Source note | uspto-grants-2001_06 |