Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Stannous Chloride | HCID 24479 | — |
| Edukt | Methyl 4-hydroxy-3-iodo-5-nitrobenzoate | HCID 21086206 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | Methyl 3-amino-4-hydroxy-5-iodobenzoate | HCID 21086158 | 92,2% |
Reaktionsschritte
To a mixture of methyl 4-hydroxy-3-iodo-5-nitrobenzoate (2.99 g) in ethanol (40 mL) was added tin (II) chloride (10 g) portion wise. After stirring for 1 h at reflux, the mixture was cooled to 0° C. and quenched by saturated potassium carbonate (100 mL). The mixture was filtered through diatomaceous earth and the filtrate was extracted with ethyl acetate (4×100 mL). The combined organic extracts were dried (sodium sulfate), filtered, and concentrated under reduced pressure to give 2.5 g of the title compound: 1H NMR (300 MHz, DMSO-d6) δ 7.50, 7.24, 3.75.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07176242B2 |
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| Quelldatensatz | uspto-grants-2007_02 |
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| ORD ID | ord-851b94af2d2c479b9347162da1c190d6 |
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| Quellennotiz | uspto-grants-2007_02 |
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