HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 1-(4-Bromo-2-nitro-phenoxy)-cyclopropanecarboxylic acid ethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 15-Crown-5 | HCID 36336 | — |
| Edukt | Ethyl 1-hydroxycyclopropane-1-carboxylate | HCID 2733706 | — |
| Edukt | 4-Bromo-3-fluoro-2-nitrophenol | HCID 53404876 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1-(4-Bromo-2-nitro-phenoxy)-cyclopropanecarboxylic acid ethyl ester | HCID 58340784 | 51,9% |
Reaktionsschritte
To a stirred solution of ethyl-1-hydroxycyclopropane carboxylate (2.93 g, 20.5 mmol) in THF (50 mL) was added sodium hydride (60% in mineral oil, 981 mg, 24.5 mmol) under argon atmosphere. After 10 min, 15-crown-5 (0.2 mL) followed by 4-bromo-2-nitro-fluorophenol (4.5 g, 20.5 mmol) were added. The reaction mixture was stirred at room temperature overnight then quenched by the addition of methanol (1.5 mL) and diluted with ethyl acetate. The mixture was washed with brine, and the organic layer was dried over anhydrous sodium sulfate, concentrated and purified by silica gel column chromatography to give 1-(4-bromo-2-nitro-phenoxy)-cyclopropanecarboxylic acid ethyl ester (3.51 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08828951B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-b015f7ca02f54c3cb9caa1ce1e96bd8e |
| Quellennotiz | uspto-grants-2014_09 |