HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 54222911, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Bromo-2-methylpropanamide | HCID 101235 | — |
| Reactant | HCID 54420518 | HCID 54420518 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 54222911 | HCID 54222911 | 94% |
Reaction Steps
Sodium hydride (10.8 mg of a 60% dispersion in oil, 0.27 mmol) was added to a solution of the phenol prepared in example 91 (100 mg, 0.25 mmol) in dry dioxane (1 ml) and the mixture stirred for 1 h at room temperature. 2-Bromo-2-methylpropanamide(Coutts, I.G.C., Southcott, M. R. J. Chem. Soc. Perkin Trans. 1, 1990, 767) was then added and the mixture heated at 100° C. for 8 h. The reaction mixture was filtered, concentrated in vacuo, and purified by flash chromatography (1:1 ethyl acetate: hexanes) to afford a light yellow solid (94.4 mg, 94%). MS (FD+) 489.6, Mp 84-86° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06413991B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-9f5e19a7d4fa435f8a9d28042c7c9367 |
| Source note | uspto-grants-2002_07 |