HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 6-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,3-Dihydro-1,4-benzodioxin-6-ol | HCID 9115273 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine | HCID 10909918 | — |
Reaction Steps
3 g (18.05 mmol) of the alcohol obtained in Step A are dissolved in 10 ml of DMF in a flask. 2 eq. of NaH (60% in oil) are added slowly and allowed to act for 30 minutes under an inert atmosphere. 2 eq. of iodomethane are then added. The mixture is stirred for 2 hours; the DMF is then evaporated. Washing with ethyl acetate and with water is carried out and the two phases are separated. The combined organic phases are dried over MgSO4 and the solvent is evaporated. The oil obtained is purified on a silica column (eluant: PE/AcOEt 8/2), which allows the pure title product to be obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313160B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-235576a5bb8949a69272b238d622c72f |
| Source note | uspto-grants-2001_11 |