HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
alpha-Ethynylbenzenemethanol → Ethyl 5-(hydroxy(phenyl)methyl)isoxazole-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | alpha-Ethynylbenzenemethanol | HCID 20155 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 2-Chloro-2-hydroxyiminoacetic acid ethyl ester | HCID 9576005 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Ethyl 5-(hydroxy(phenyl)methyl)isoxazole-3-carboxylate | HCID 66831982 | 70% |
Reaktionsschritte
1-phenylprop-2-yn-1-ol (0.802 mL, 6.60 mmol) was added to a mixture of (Z)-ethyl 2-chloro-2-(hydroxyimino)acetate (0.50 g; 3.30 mmol) and sodium hydrogen carbonate (0.554 g; 6.60 mmol) in ethyl acetate (15 mL) and water (0.2 mL) and stirred at room temperature for 24 hours. The resulting mixture was filtered and concentrated under reduced pressure. The crude mixture was purified by flash chromatography on silica (eluent 2 to 40% ethyl acetate in heptane) to yield 0.571 g (70%) of ethyl 5-(hydroxy(phenyl)methyl)isoxazole-3-carboxylate as a colorless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09434722B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-ef0452aa01e04e21813141893bd989e4 |
| Quellennotiz | uspto-grants-2016_09 |