HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Acetate → HCID 178428410, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | dihydrothiophen-3(2H)-one 1,1-dioxide | HCID 5150067 | — |
| Reactant | HCID 178467936 | HCID 178467936 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178428410 | HCID 178428410 | — |
Reaction Steps
850 mg (6.336 mmol) dihydrothiophen-3(2H)-one-1,1-dioxide, 1.78 g (6.336 mmol) (2E)-2-[(3-methyl-1H-indazol-5-yl)methylidene]-3-oxobutanenitrile (Example 2A) and 586 mg (7.603 mmol) ammonium acetate in acetic acid (30 ml) were heated to reflux overnight. After cooling, the mixture was evaporated to dryness, and the residue was taken up in ethyl acetate and washed with water and brine. The organic layer was separated and dried over sodium sulfate. After filtration and evaporation to dryness, the remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient) to yield 89 mg (4% 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-f88c981ad8ac4ee18966994417f4a0b9 |
| Source note | uspto-grants-2014_06 |