HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 5-(1-Hydroxy-2-methylprop-2-enyl)furan-2-carboxylic acid benzyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 5-Formyl-2-furancarboxylic acid benzyl ester | HCID 60034788 | — |
| Edukt | HCID 178455850 | HCID 178455850 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 5-(1-Hydroxy-2-methylprop-2-enyl)furan-2-carboxylic acid benzyl ester | HCID 86673322 | 94,6% |
Reaktionsschritte
5-Formyl-2-furancarboxylic acid benzyl ester (300 mg, 1.30 mmol) was dissolved in tetrahydrofuran (12 mL), 2-propenylmagnesium bromide (0.5 mol/L tetrahydrofuran solution, 2.6 mL, 1.3 mmol) was added at −78° C., and the mixture was stirred for 15 minutes. 1N Hydrochloric acid was added to the reaction mixture, the mixture was heated to room temperature and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=70/30) to give the title compound (332 mg, 1.23 mmol, 94%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08877805B2 |
| Quelldatensatz | uspto-grants-2014_11 |
| ORD ID | ord-6bb6b5833c3f4160919148895af1c4d5 |
| Quellennotiz | uspto-grants-2014_11 |