HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine, dihydrochloride → HCID 178469268, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine, dihydrochloride | HCID 17548 | — |
| Reactant | Ethyl 4-(dimethylamino)-2-oxo-but-3-enoate | HCID 2777802 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178469268 | HCID 178469268 | 39% |
Reaction Steps
4-Dimethylamino-2-oxo-but-3-enoic acid ethyl ester (195 g, 1.14 mol) and hydrazine dihydrochloride (119.7 g, 1 eq) were dissolved in EtOH (1 L) and stirred at room temperature overnight. The mixture was then heated to reflux for 2 hours. The reaction mixture was allowed to cool to room temperature and filtered. The solid was washed with water three times and dried. The filtrate was concentrated to a thick oil and added dropwise into a flask with stirred EtOAc (200 mL). The resulting solid was filtered and rinsed with a small amount of EtOAc. The filtered solids were combined to give the product (62 g, 39% yield). MS (ES) m/z 141.1 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853202B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-911aa2f3c08b48569e37d059fdd4f59c |
| Source note | uspto-grants-2014_10 |