Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 6-Bromo-4-cinnolinol | HCID 270902 | — |
| Produkt | 6-Bromo-4-chlorocinnoline | HCID 12448078 | 43% |
Reaktionsschritte
A solution of Example 34C (0.4 g, 1.8 mmol) in POCl3 (2.5 mL) was heated to 100° C. for 2 hours, and poured slowly onto ice. The aqueous layer was cooled to 0° C. and adjusted to pH 5-7 with 50% NaOH. The aqueous layer was extracted with ethyl acetate (2×50 mL), and the combined organic layers were concentrated. The residue was purified by flash column chromatography on silica gel with 4:1 hexanes/ethyl acetate to provide the desired product (0.190 g, 43%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06831175B2 |
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| Quelldatensatz | uspto-grants-2004_12 |
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| ORD ID | ord-8e45b3c3aee24d2191646d7def1850e8 |
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| Quellennotiz | uspto-grants-2004_12 |
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