Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethyl Acetoacetate | HCID 8868 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Edukt | 3-Bromo-2-Methoxyaniline hydrochloride | HCID 86810414 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178472845 | HCID 178472845 | — |
Reaktionsschritte
To a solution of 3-bromo-2-methoxyaniline hydrochloride (10 g) prepared as in Example 15, in hydrochloric acid (13.5 mL of concentrated hydrochloric acid in 136.5 mL of water) was added a solution of sodium nitrite (3.47 g in 10 mL of water) at about −5° C. to about 5° C. under stirring. The reaction mixture was stirred for about 1 hour at about −5° C. to about 5° C. Then ethylacetoacetate (6.55 g) was added to the reaction mixture and stirred for about 3 hours at about −5° C. to about 5° C. Sodium bicarbonate and methanol was then added to the reaction mixture. The reaction mixture was stirred at about −5° C. to about 5° C. for about 1 hour. The mixture was filtered to give a solid, which was washed with water and dried at about 50° C. to about 55° C. Yield: 13.3 g
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09440927B2 |
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| Quelldatensatz | uspto-grants-2016_09 |
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| ORD ID | ord-e250670b322b43899edd2e2071c6b71d |
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| Quellennotiz | uspto-grants-2016_09 |
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