HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Acetate → HCID 178428415, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 4-hydroxy-5,5-dimethyl-1,5-dihydro-2H-pyrrol-2-one | HCID 66725429 | — |
| Reactant | HCID 178467936 | HCID 178467936 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178428415 | HCID 178428415 | — |
Reaction Steps
A solution of 200 mg (0.888 mmol) (2E)-2-[(3-methyl-1H-indazol-5-yl)methylidene]-3-oxobutanenitrile (Example 2A), 226 mg (0.888 mmol, approx. 50% purity) 4-hydroxy-5,5-dimethyl-1,5-dihydro-2H-pyrrol-2-one [K. Matsuo et al., Chem. Pharm. Bull. 1984, 32, 3724-3729] and 102 mg (1.332 mmol) ammonium acetate in acetic acid (4 ml) was stirred at 100° C. for 15 min. The reaction mixture was concentrated under reduced pressure, and the residue was purified first by preparative RP-HPLC (acetonitrile/water+0.1% TFA gradient) and then by preparative TLC (eluent: dichloromethane/methanol 10:1) to give 33 mg (11% of th.) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759341B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-27d280bf61cd4c2db159f8f46ec36947 |
| Source note | uspto-grants-2014_06 |