HuagongsheHuagongshe Chemistry Print Report · For research reference only
Coumaranone → Benzofuran-3-acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Coumaranone | HCID 23556 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Benzofuran-3-acetonitrile | HCID 2769401 | 91% |
Reaction Steps
Sodium hydride (268 mg, 6.7 mmol) was slurried in dry THF (10 ml) at 0° C. under nitrogen and diethyl cyanomethyl phosphonate (1.1 ml, 6.7 mmol) added dropwise and the whole stirred for 45 min. 3-Coumaranone (Lancaster) (900 mg, 6.7 mmol) was then added dropwise and the whole stirred at room temperature for 45 min. The reaction was diluted with EtOAc (15 ml) and water (15 ml), and the organic layer was then separated, dried (MgSO4) and evaporated and the residue flash chromatographed using 0-5% EtOAc in pentane to give the title product (940 mg, 91%); 1HNMR (400 MHz, CDCl3) δ: 3.77 (s, 2H), 7.25-7.40 (m, 2H), 7.52 (dd, 1H), 7.58 (dd, 1H), 7.67 (s, 1H); LRMS: M+NH4+, 175. (TS+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06660756B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-dcf6a7a44a134677af4f3871218f3b28 |
| Source note | uspto-grants-2003_12 |