HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 5-Hydroxy-3-phenyl-5-(trifluoromethyl)-4,5-dihydroisoxazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4,4,4-Trifluoro-1-phenyl-1,3-butanedione | HCID 67589 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Product | 5-Hydroxy-3-phenyl-5-(trifluoromethyl)-4,5-dihydroisoxazole | HCID 2880976 | 91.5% |
Reaction Steps
Prepared according to J. Org. Chem., 1995, 60, 3907. A solution of benzoyltrifluoroacetone (21 g, 97 mmol) was added dropwise over 1 h, at 20-30° C., to a solution of hydroxylamine HCl (6.82 g, 98 mmol) containing sodium hydroxide (2 N, 51 mL, 102 mmol) and the resulting mixture heated under reflux for 45 min. After cooling to room temperature, the mixture was poured into ice-water (500 mL), the precipitate was filtered off, washed with water and dried under vacuum to afford the title compound (20.51 g, 91%) which was obtained as a white solid. MS: m/e=230.2 [M−H]−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846719B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-f1bc98c06fe04b62b2e9262b0f153135 |
| Source note | uspto-grants-2014_09 |