Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 3-Chloro-5-nitrophenol | HCID 10675815 | — |
| Katalysator | Zinc | HCID 23994 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Amino-5-chlorophenol | HCID 19986947 | 79,3% |
Reaktionsschritte
3-Chloro-5-nitrophenol from Example 63A (3.00 g, 17.3 mmol) and zinc powder (5.65 g, 86.4 mmol) in ethanol (80 mL) were heated to 60° C., and a solution of ammonium chloride (1.85 g, 34.6 mmol) in water (16 mL) was added dropwise. The reaction was stirred for further 3 h at 60° C. It was then filtered through Celite®, and the solvent was removed in vacuo. The residue was dissolved in water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo. The residue was triturated with DCM, and the precipitate was collected by suction filtration to yield 1.97 g (77%) of the title compound as yellowish crystals.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08524722B2 |
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| Quelldatensatz | uspto-grants-2013_09 |
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| ORD ID | ord-2499ae564da64b81bf11c0ce6a6c971f |
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| Quellennotiz | uspto-grants-2013_09 |
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