HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-Bromo-1,2-benzoxazol-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2-Bromo-6-fluorobenzonitrile | HCID 2783139 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Product | 4-Bromo-1,2-benzoxazol-3-amine | HCID 45588471 | — |
Reaction Steps
A suspension of acetylhydroxamic acid (2.46 g, 32.8 mmol) and potassium tert-butoxide (3.68 g, 32.8 mmol) in DMF (40 mL) was stirred at room temperature for 30 minutes, treated with 2-bromo-6-fluorobenzonitrile (4.36 g, 21.8 mmol), stirred for three hours, poured into water, and extracted three times with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated. The residue was purified by flash column chromatography on silica gel with 5 to 20% ethyl acetate/hexanes to provide 2.5 g of the desired product. MS (ESI(+)) m/e 212.9, 214.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063091B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-c07c1ce3eacd4d46a398df1834c79bd2 |
| Source note | uspto-grants-2011_11 |