HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66906323, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (2,6-Dichlorophenyl)hydrazine monohydrochloride | HCID 2723909 | — |
| Reactant | HCID 66906104 | HCID 66906104 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 66906323 | HCID 66906323 | 37.8% |
Reaction Steps
To a solution of 3-cyclopropyl-4-dimethylamino-2-oxo-but-3-enoic acid ethyl ester (6.5 mmol, 1.4 g) in ethanol (25 mL) is added 2,6-dichlorophenyl hydrazine hydrochloride (7.2 mmol, 1.5 g) followed by concentrated HCl (100 μL). The reaction is stirred for 4 h at room temperature followed by heating at 85° C. for 18 h. The reaction mixture is adsorbed onto silica gel and purified using a gradient of 0-20% EtOAc/Hexanes to yield the title compound (0.8 g, 34%). LC-ES/MS m/e 325.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153624B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-5c856782ba9b45f19676d627d2b2b03f |
| Source note | uspto-grants-2012_04 |