Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate | HCID 22328992 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 22329314 | HCID 22329314 | 82,6% |
Reaktionsschritte
In THF (5.0 ml)/methanol (5.0 ml) was dissolved methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate (0.50 g). To the solution was added 2N potassium hydroxide (5.0 ml), and the mixture was stirred at 50° C. for 3 hours. pH was adjusted to approximate 4 with 6N hydrochloric acid, and the solvent was concentrated to half under reduced pressure. The concentrated material was extracted with ethyl acetate, and the extract was washed with saturated brine and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was washed with hexane/ethyl acetate (=8/1) to give 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylic acid (0.40 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06936602B1 |
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| Quelldatensatz | uspto-grants-2005_08 |
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| ORD ID | ord-9809f2f518ca424c9051686931b90cab |
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| Quellennotiz | uspto-grants-2005_08 |
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