HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 69138960, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acetoxyacetyl chloride | HCID 26297 | — |
| Reactant | HCID 178492247 | HCID 178492247 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69138960 | HCID 69138960 | 80.4% |
Reaction Steps
A solution (2.29 l) of N-[(E)-(3-fluoro-2-pyridyl)methylidene]-4-methoxyaniline (449 g) and triethylamine (204 g) in dichloromethane was cooled to −10° C. Then acetoxyacetyl chloride (250 g) was added dropwise thereinto and the resultant mixture was stirred at the same temperature for 30 minutes. Then it was heated to room temperature and stirred for 16 hours. The liquid reaction mixture was washed with water and the solvent was concentrated under reduced pressure to thereby give a crude product (723 g). This crude product was recrystallized from a solvent mixture of ethanol (6.9 l) and ethyl acetate (350 ml) to thereby give the title compound (486 g) as brown crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07126003B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-4b62c541b8594a209f15c12f81e510f8 |
| Source note | uspto-grants-2006_10 |