Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Methyl 5-bromo-2-methyl-3-nitrobenzoic acid | HCID 86623945 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Methyl 3-bromo-5-nitrobenzoate | HCID 239341 | 104,6% |
Reaktionsschritte
To stirred solution of 5-bromo-2,4-dimethyl-3-nitrobenzoic acid (13 g, 47.44 mmol) in DMF (120 mL), sodium carbonate (15 g, 142.2 mmol) and methyl iodide (4.4 ml, 71.16 mmol) were added. Resulting reaction mass was heated at 60° C. for 8 h. On completion, water was added to the reaction mass and extraction was carried out using ethyl acetate. Combined organic layers were washed with sat. bicarbonate solution and 5 N HCl, dried over sodium sulphate, concentrated under reduced pressure giving desired compound (12.9 g, 86%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09376422B2 |
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| Quelldatensatz | uspto-grants-2016_06 |
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| ORD ID | ord-bf978c14db984630b8147a13eb9148b8 |
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| Quellennotiz | uspto-grants-2016_06 |
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