HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hexane → 2-(2-Bromoethyl)-3-(bromomethyl)thiophene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hexane | HCID 8058 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 2-(3-Hydroxymethylthiophen-2-yl)ethanol | HCID 11182761 | — |
| Edukt | Triphenylphosphane dibromide | HCID 12890784 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-(2-Bromoethyl)-3-(bromomethyl)thiophene | HCID 69311722 | 80,8% |
Reaktionsschritte
2.0 g of the compound obtained in Example 2 was dissolved in 40 mL of dichloromethane, and the resulting solution was cooled to below 5° C. 13.4 g of triphenylphosphine dibromide was added thereto, and the resulting mixture was warmed to room temperature, stirred for 4 hours, and concentrated by evaporation under reduced pressure. To the residue, 5 mL of ethyl acetate and then 15 mL of n-hexane were added. The resulting mixture was stirred for 1 hour at room temperature and 2 hours at below 5° C., filtered and condensed under reduced pressure. The residue was subjected to silica gel column chromatography (eluent, n-hexane:ethyl acetate=10:1) to obtain 2.9 g (yield of 80%) of the title compound as a yellowish oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07449580B2 |
| Quelldatensatz | uspto-grants-2008_11 |
| ORD ID | ord-7b9e97b820d749ef97db4a66cf0bbc7f |
| Quellennotiz | uspto-grants-2008_11 |