HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetoacetate → Ethyl 2-{4-[15-(trifluoromethyl)pentadecylamino]benzoyl}acetoacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-[15-(Trifluoromethyl)pentadecylamino]benzoyl chloride hydrochloride | HCID 20549317 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | Ethyl 2-{4-[15-(trifluoromethyl)pentadecylamino]benzoyl}acetoacetate | HCID 20549413 | — |
Reaction Steps
A solution of 21.6 g. of ethyl acetoacetate and 10 ml. of 1,2-dimethoxyethane is added to a suspension of 4.0 g. of sodium hydride in 1,2-dimethoxyethane under argon. A solution of 17.3 g. of 4-[15-(trifluoromethyl)pentadecylamino]benzoyl chloride hydrochloride in 1,2-dimethoxyethane is then added. The reaction mixture is refluxed for 5 hours, cooled, poured on ice and extracted with ether. The ether solution is washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated to dryness. Recrystallization from ether affords the product as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04318914 |
| Source dataset | uspto-grants-1982_03 |
| ORD ID | ord-aef223dd389f46439e0f3f05867b0e8d |
| Source note | uspto-grants-1982_03 |