HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 4-chloroacetoacetate → HCID 86683109, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Reactant | 2-Amino-4-fluoropyridine | HCID 18327808 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86683109 | HCID 86683109 | 17.7% |
Reaction Steps
A mixture of 4-fluoropyridin-2-amine (1.0 g, 8.92 mmol) and ethyl 4-chloro-3-oxobutanoate (1.46 mL, 10.7 mmol) in THF (20 mL) was stirred at about reflux overnight. The residue was concentrated and was chromatographed on the C18 ISCO Combiflash system using the following gradient: A: Water (0.1% NH4HCO3); B: Methanol; 10% B to 60% B over 20 min to give 350 mg product as brown oil (350 mg, yield: 17.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273068B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-6ebfe3e6652242c38d1910421a6138aa |
| Source note | uspto-grants-2016_03 |