Sodium hydride → 5,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one
Reaktionsgleichung
[H-].[Na+].Br[C:4]1[C:9]([NH:10][C:11]([C:13]2[C:14]([NH:19][CH2:20][CH3:21])=[N:15][CH:16]=[CH:17][CH:18]=2)=[O:12])=[C:8]([CH3:22])[CH:7]=[C:6]([O:23][CH3:24])[N:5]=1>N1C=CC=CC=1.C(OCC)(=O)C>[CH2:20]([N:19]1[C:14]2[N:15]=[CH:16][CH:17]=[CH:18][C:13]=2[C:11](=[O:12])[NH:10][C:9]2[C:8]([CH3:22])=[CH:7][C:6]([O:23][CH3:24])=[N:5][C:4]1=2)[CH3:21]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
Sodium hydride (0.14 g of a 50% dispersion in mineral oil) was added to a solution of N-(2-bromo- 6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide (0.54 g) in pyridine (4 ml), and the resulting mixture was refluxed for 1.5 hours. The cooled mixture was diluted with ethyl acetate, washed with water, and the organic phase was dried (anhydrous magnesium sulfate) and concentrated. The residue was washed with diisopropyl ether and hot ethyl acetate, and then crystallized from ethanol to provide 0.2 g of 5,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one m.p. 249°-251° C.
Aufarbeitung
- temperaturethe resulting mixture was refluxed for 1.5 hours
- washwashed with water
- dry with materialthe organic phase was dried (anhydrous magnesium sulfate)
- concentrationconcentrated
- washThe residue was washed with diisopropyl ether and hot ethyl acetate
- customcrystallized from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-dc2d6d466d6840ce9a7ab52ddb87b348
- Quelldatensatz
- uspto-grants-1994_11
- Patentnummer
- US05366972
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