Reaktion #81811

Reaktionsgleichung

Sodium hydride

N-(2-bromo-6-methoxy-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

→

5,11-dihydro-11-ethyl-2-methoxy-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

Ausbeute 47.6%

Lösungsmittel

ethyl acetate

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe resulting mixture was refluxed for 1.5 hours
2. 2
   Waschenwashed with water
3. 3
   Trocknenthe organic phase was dried (anhydrous magnesium sulfate)
4. 4
   Einengenconcentrated
5. 5
   WaschenThe residue was washed with diisopropyl ether and hot ethyl acetate
6. 6
   Sonstigecrystallized from ethanol

Vorschrift

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.

Quelle