Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chloroform | HCID 6212 | — |
| Edukt | 2-Fluoro-5-nitrobenzotrifluoride | HCID 94954 | — |
| Edukt | Acetic acid methanol | HCID 10129899 | — |
| Edukt | Potassium tert-butoxide | HCID 23665647 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | Sodium chloride; water | HCID 57417360 | — |
| Produkt | HCID 18536748 | HCID 18536748 | 51,2% |
Reaktionsschritte
To a solution of potassium t-butoxide (1.25 g, 11.1 mmol) in tetrahydrofuran (25 ml) was slowly added dropwise a solution of 2-fluoro-5-nitrobenzotrifluoride (1.00 g, 4.78 mmol) and chloroform (599 mg, 5.02 mmol) in tetrahydrofuran (2.5 ml) at −78° C. After stirring for 15 minutes at the same temperature, acetic acid-methanol (1:1, 5 ml) was added and the temperature was raised to room temperature. Ethyl acetate and saturated brine were added to the reaction mixture, which was extracted with ethyl acetate. After washed with brine, the organic layer was dried over anhydrous magnesium sulfate and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [hexane→hexane-ethyl acetate(300:1)] to obtain 714 mg of title compound as pale yellow liquid. Yield 51%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06562839B1 |
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| Quelldatensatz | uspto-grants-2003_05 |
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| ORD ID | ord-709a237c3984425b80c000aa069b163e |
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| Quellennotiz | uspto-grants-2003_05 |
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