HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 22321557, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 4-Amino-1(2H)-phthalazinone | HCID 595178 | — |
| Reactant | HCID 22321558 | HCID 22321558 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22321557 | HCID 22321557 | 43% |
Reaction Steps
4-Amino-1-phthalazinone (2.28 g, 14.2 mmol) [Angew. (1967) 6(2) 173-4] and 2-hydroxy-1-(5-methylisoxazol-3-yl)ethanone (2.0 g, 14.2 mmol) were suspended in toluene (100 ml) and trifluoroacetic acid (5 ml) was added. The suspension was heated at reflux under Dean & Stark conditions, for 24 hours. The solvent was then removed in vacuo and the residue was purified by chromatography on silica gel eluting with 10% methanol:dichloromethane, to provide the title product (1.62 g, 43%), 1H NMR (360 MHz, d6-DMSO) 2.50 (3H, s), 5.96 (2H, br s), 7.79-8.22 (4H, m) 11.48 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06946461B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-e28354f1c9d44c1db0a0965ef092bfaa |
| Source note | uspto-grants-2005_09 |