HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 53517Erstellt: 25. Oktober 2026
Sodium hydride → 11-Ethyl-4-trifluoromethyl-2-methyl-5H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6(11H)-one
https://huagongshe.com/reaction/53517
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
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| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | N-(2-chloro-6-methyl-4-trifluoromethyl-3-pyridinyl)-2-ethylamino-3pyridinecarboxamide | HCID 19960041 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 11-Ethyl-4-trifluoromethyl-2-methyl-5H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6(11H)-one | HCID 15221251 | 20% |
Reaktionsschritte
A solution of 0.5 g of N-(2-chloro-6-methyl-4-trifluoromethyl-3-pyridinyl)-2-ethylamino-3pyridinecarboxamide in 3 ml of pyridine was added to 0.2 g of a 50% dispersion of sodium hydride in oil. The mixture was heated to 150° C. and then cooled and concentrated in vacuo. Water was added to the residue and the product was extracted with ethyl acetate, dried (magnesium sulfate), filtered, and concentrated. The product was purified by column chromatography over silica gel (methylene chloride, then methylene chloride/methanol). After concentrating in vacuo, the residue was crystallized from hexane to give 0.09 g of the title compound, m.p. 150°-151° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05620974 |
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| Quelldatensatz | uspto-grants-1997_04 |
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| ORD ID | ord-fb65b49f987f4ae2b0bd18991deb0d31 |
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| Quellennotiz | uspto-grants-1997_04 |
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