HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylsilane → 6-(2-Bromo-5-iodobenzyl)-2,3-dihydrobenzo[b][1,4]dioxine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylsilane | HCID 12052 | — |
| Edukt | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Edukt | Methanone, (2-bromo-5-iodophenyl)(2,3-dihydro-1,4-benzodioxin-6-yl)- | HCID 58340798 | — |
| Lösungsmittel | Trifluoroacetic acid | HCID 6422 | — |
| Produkt | 6-(2-Bromo-5-iodobenzyl)-2,3-dihydrobenzo[b][1,4]dioxine | HCID 58340830 | 91,2% |
Reaktionsschritte
To a stirred solution of (2-bromo-5-iodo-phenyl)-(2,3-dihydro-benzo[1,4]dioxin-6-yl)-methanone (30.0 g, 67.4 mmol) in trifluoroacetic acid (100 mL) was added triethylsilane (86.2 mL, 539.3 mmol) followed by triflic acid (6.0 mL, 67.42 mmol) at room temperature. After stirring for 25 min at room temperature, volatiles were evaporated under reduced pressure. The resulting residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution (200 mL×2), water (200 mL), and brine (200 mL), then dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 6-(2-bromo-5-iodo-benzyl)-2,3-dihydro-benzo[1,4]dioxine (26.5 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08828951B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-1807c45f54754e01adefbce5d50c9cab |
| Quellennotiz | uspto-grants-2014_09 |