HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178469356, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Diethyl acetylenedicarboxylate | HCID 69803 | — |
| Reactant | 2-Fluoro-3-hydrazinylpyridine | HCID 55280945 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178469356 | HCID 178469356 | 34% |
Reaction Steps
To a solution of 2-fluoro-3-hydrazinopyridine (30.0 g) in ethanol (472 mL) were added sodium carbonate (65.2 g) and diethyl but-2-ynedioate (40.2 g). After refluxing for 18 hr, the mixture was cooled to room temperature, treated with 2 mol/L hydrochloric acid, and extracted twice with ethyl acetate. The extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was suspended in diethyl ether, and the obtained solid was collected by filtration and dried under reduced pressure to give the title compound as a yellow solid (yield 20.0 g, yield 34%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895588B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-3303946d6dc64b3382b0c9c5a1935f23 |
| Source note | uspto-grants-2014_11 |