Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methyl 4-fluoro-2-(methylamino)benzoate | HCID 13474393 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Edukt | HCID 178434708 | HCID 178434708 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Produkt | HCID 178482227 | HCID 178482227 | — |
Reaktionsschritte
A solution of butyl lithium in hexane (2.7M, 53 ml) was added to a stirred suspension of 5-methyltetrazole (6.0 g) in dry tetrahydrofuran (250 ml) at 0° under nitrogen. A solution of methyl 4-fluoro-2-methylaminobenzoate (4.36 g) in dry tetrahydrofuran (20 ml) was added during 10 minutes. The mixture was stirred for 17 hours at room temperature and then for 3 hours at 40° to 70°. The mixture was cooled to room temperature and water (200 ml) was added. The mixture was neutralised with dilute aqueous hydrochloric acid and extracted with dichloromethane (3×100 ml). The combined extracts were dried and evaporated under reduced pressure. The residue was crystallised from industrial methylated spirit to give the novel compound 1-(4-fluoro-2-methylaminophenyl)-2-(1H-tetrazol-5-yl)ethanone, m.p. 214°-6°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04659718 |
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| Quelldatensatz | uspto-grants-1987_04 |
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| ORD ID | ord-6789cd0c6d0b42eb9df4ab2d67874bfc |
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| Quellennotiz | uspto-grants-1987_04 |
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