Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 2,6-Dimethylphenol | HCID 11335 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-(2',6'-Dimethylphenoxy)phthalonitrile | HCID 952073 | 87% |
Reaktionsschritte
A mixture of 4-nitro-phthalonitrile (1 eq), 2,6-dimethylphenol (1.2 eq), K2CO3 (2 eq), and DMF (1 mL/mmol 4-nitro-phthalonitrile) was heated under nitrogen at 60° C. for 3 h with stirring. After cooling to ambient temperature the mixture was poured into water (6 mL/mL DMF) with stirring. The mixture was extracted twice with EtOAc. The combined organic phases were dried over MgSO4 and concentrated in vacuo. The residue was recrystallized from EtOH to give the title compound as a tan solid (yield: 87%); 1H NMR (CDCl3, 200 MHz): δ=7.70 (d, 1H), 7.05 to 7.16 (m, 5H), 2.08 (s, 6H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09174976B2 |
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| Quelldatensatz | uspto-grants-2015_11 |
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| ORD ID | ord-3eaf6c55f8e84abc82d5bd711741b9d7 |
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| Quellennotiz | uspto-grants-2015_11 |
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