Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Ammonium Hydroxide | HCID 14923 | — |
| Edukt | Thionyl Chloride | HCID 24386 | — |
| Edukt | 2-Amino-3-nitrobenzoic acid | HCID 219633 | — |
| Lösungsmittel | 1,2-Dimethoxyethane | HCID 8071 | — |
| Produkt | 2-Amino-3-nitrobenzamide | HCID 10797476 | 89% |
Reaktionsschritte
To a solution of 2-amino-3-nitrobenzoic acid (prepared using the procedure as described in U.S. Pat. No. 6,737,421, EXAMPLE 2, part b) in dimethoxyethane (DME, 7.1 mL/g), was added thionyl chloride (1.33 equivalents). The mixture was stirred at 50° C. for 12 hours, cooled and slowly added to concentrated ammonium hydroxide (22 equivalents). The mixture was stirred at 50° C. for 2 hours, water was added, and the mixture was cooled and filtered. The solid was washed with water and isopropanol, and dried under vacuum to give the title compound (89% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07595406B2 |
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| Quelldatensatz | uspto-grants-2009_09 |
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| ORD ID | ord-10723559ed7945fd884e11a711969e85 |
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| Quellennotiz | uspto-grants-2009_09 |
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