HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 5-Bromo-2,2-dimethyl-2,3-dihydro-1-benzofuran
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2,3-Dihydro-2,2-dimethylbenzofuran | HCID 80640 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | 5-Bromo-2,2-dimethyl-2,3-dihydro-1-benzofuran | HCID 219475 | 79% |
Reaction Steps
2,2-Dimethyl-2,3-dihydrobenzo[b]furan (prepared according to the method of Baker and Shulgin, J. Org. Chem., 28, 1963, 2468) (500 mg, 3.38 mmol) was taken up in dichloroethane (5.5 ml) and stirred at room temperature under nitrogen, and N-bromosuccinimide (661 mg, 3.72 mmol) added in one portion. The reaction was then refluxed for 2 h, ether was added (10 ml) and a white precipitate of succinimide filtered off. The filtrate was evaporated to dryness, and then purified by column chromatography using 5% ether in pentane as eluant to give the title product (604 mg, 79%); 1HNMR (400 MHz, CDCl3) δ: 1.43 (s, 6H), 2.92 (s, 2H), 6.54 (d, 1H), 7.16 (d, 1H), 7.19 (s, 1H); LRMS: M+H, 227. (TS+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06660756B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-8cca403ca0b94291abad41bee111fcb1 |
| Source note | uspto-grants-2003_12 |