HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 5-[2-(methylthio)phenyl]-1H-indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-Bromothioanisole | HCID 88166 | — |
| Reactant | 5-Indolylboronic acid | HCID 2734361 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 5-[2-(methylthio)phenyl]-1H-indole | HCID 12148820 | 52.2% |
Reaction Steps
A solution of 5-indoleboronic acid (2.0 g, 12 mmol) and 2-bromothioanisole (1.6 mL, 12 mmol) in a mixture of ethylene glycol dimethyl ether (20 mL) and aqueous sodium carbonate (10 mL) was deoxygenated by a rapid stream of nitrogen applied to the system for 20 min, then treated with Pd(0) at once. The reaction was refluxed for 18 h, cooled down, filtered through Celite® and washed with THF (20 mL). The filtrate evaporated to dryness, taken up in water and extracted with EtOAc (3×). The EtOAc extracts were dried over sodium sulfate and concentrated. The crude residue was purified by flash chromatography (hexane/EtOAc, 1:3) to afford 5-[2-(methylthio)phenyl]-1H-indole (1.5 g, 52%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06429205B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-8bec870de9de44de863af34bf55ebd08 |
| Source note | uspto-grants-2002_08 |