HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 178434567, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | HCID 86711960 | HCID 86711960 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178434567 | HCID 178434567 | 44.3% |
Reaction Steps
To a solution of 5-(4-(trifluoromethoxy)phenyl)isoxazole-3-carbohydrazide (4.4 g, 15.3 mmol) and acetimidamide hydrochloride (2.2 g, 23.0 mmol) in dry THF (100 mL) was added NaOH (920 mg, 23.0 mmol), and the resulting mixture was refluxed for 16 h. The solution was then cooled to RT and concentrated under reduced pressure, the residue was partitioned between H2O (80 mL) and EtOAc (2×100 mL). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography (Petroleum ether:EtOAc=1:2) to afford the title compound as a yellow solid (2.1 g, 44.3%). MS (ES+) C13H9F3N4O2 requires: 310. found: 311 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018380B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-2ae841196587422ea9920767481b81c8 |
| Source note | uspto-grants-2015_04 |