HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15384498, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 3-Acetyl-2,4-dimethylfuran | HCID 579676 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 15384498 | HCID 15384498 | 88% |
Reaction Steps
A mixture of 3-acetyl-2,4-dimethylfuran (commercially available from Aldrich Chemical Co., Inc., 1 g, 7.24 mmol), N-bromosuccinimide (NBS; 1.3 g, 7.3 mmol), and 2,2'-azobisisobutyronitrile (AIBN; 3 mg) in benzene (10 mL) was heated at reflux temperature for one hour. After cooling, water (50 mL) was added to the mixture. The whole was extracted with benzene (50 mL), the organic layer washed with water, brine, dried over MgSO4, and concentrated in vacuo. Chromatographic purification of the residue eluting with ethyl acetate-hexane (1:10) provided the subtitle compound (1.38 g, 88% yield) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06048880 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-16b69e0e5d2e4620825207db1a48e07b |
| Source note | uspto-grants-2000_04 |