HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → 4-(Hydroxy-(5-methyl-furan-2-yl)-methyl)benzaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | 5-Methylfurfural | HCID 12097 | — |
| Edukt | 1-Bromo-4-(dimethoxymethyl)benzene | HCID 688342 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4-(Hydroxy-(5-methyl-furan-2-yl)-methyl)benzaldehyde | HCID 59255336 | 12,3% |
Reaktionsschritte
To a mixture of 4-bromobenzaldehyde dimethyl acetal (2.0 mL, 12 mmol) and diethyl ether (30 mL) was added dropwise n-butyl lithium (1.6 M n-hexane solution, 9.0 mL, 14 mmol) at −78° C., which was stirred for 20 minutes at the same temperature. 5-Methylfurfural (1.3 mL, 13 mmol) was added dropwise into the reaction mixture at that temperature, and stirred for 50 minutes at 0° C. Water and ethyl acetate were added to extract the reaction mixture. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:2) to obtain the title compound (320 mg, 12%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08153662B2 |
| Quelldatensatz | uspto-grants-2012_04 |
| ORD ID | ord-1a1839b0d51345f99fe5b6801f2fd62a |
| Quellennotiz | uspto-grants-2012_04 |