HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron trifluoride etherate → HCID 13290014, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron trifluoride etherate | HCID 8000 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 13952868 | HCID 13952868 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 13290014 | HCID 13290014 | 60.9% |
Reaction Steps
A solution of 3.7 g of 6,7-dichloro-2,3-dihydro-3-hydroxy-5-methoxy-2-methylbenzo[b]thiophene in 20 ml of glacial acetic acid containing 5 ml of boron trifluoride etherate is warmed on a steam bath for 5 min. to form a clear solution. After stirring at room temperature for 1 hour, the solution is poured into an ice-cold solution of 10% sodium hydroxide. The organic materials are extracted 3 times with ether, dried and concentrated under vacuum. The reddish brown residue is purified by dissolving it in ether and passing it through an alumina column packed with ether. Elution with ether gives 2.1 g of 6,7-dichloro-5-methoxy-2-methylbenzo[b]thiophene as off-white crystals, mp 113°-114°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04436748 |
| Source dataset | uspto-grants-1984_03 |
| ORD ID | ord-39273926a4ae407189c43bfee56b904a |
| Source note | uspto-grants-1984_03 |