HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 4-chloroacetoacetate → HCID 12269134, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Reactant | 2-Amino-5-bromopyridine | HCID 70622 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 12269134 | HCID 12269134 | — |
Reaction Steps
4.90 ml of ethyl4-chloro-3-oxobutanoate was dissolved in 50 ml of ethanol, 5.19 g of 2-amino-5-bromopyridine was added, and the mixture was stirred all night by heating under reflux. After cooling down to room temperature, the solvents were distilled outunder reduced pressure, and then, ethyl acetate followed by saturated sodium bicarbonate aqueous solution were added. Organic layer was dried with anhydrous sodium sulfate, and the solvents were distilled outunder reduced pressure. The obtained residues were purified by preparative thin-layer chromatography (hexane:ethyl acetate=60:40) to obtain 9.49 mg of the above compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902369B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-0ca75aa2738a4ef5a2eaa46384bb3da2 |
| Source note | uspto-grants-2011_03 |