Reaktion #162425

Reaktionsgleichung

(2,6-Dichlorophenyl)hydrazine hydrochloride

6-[(dimethylamino)methylene]-6,11-dihydro-5H-dipyrido[2,3-b:3′,4′-f]azepin-5-one

→

desired product

2-(2,6-Dichlorophenyl)-2,8-dihydropyrazolo[3,4-d]dipyrido[2,3-b:3′,4′-f]azepine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated to 60° C. overnight
2. 2
   TemperaturThe reaction was then cooled to room temperature
3. 3
   Sonstigethe major product from the reaction mixture was isolated

Vorschrift

(2,6-Dichlorophenyl)hydrazine hydrochloride (168 mg, 0.788 mmol) was added to a solution of 6-[(dimethylamino)methylene]-6,11-dihydro-5H-dipyrido[2,3-b:3′,4′-f]azepin-5-one (105 mg, 0.394 mmol, Intermediate E-1) in ethanol (4 mL) and stirred at room temperature. After 30 minutes, the mixture was heated to 60° C. overnight. The reaction was then cooled to room temperature and the major product from the reaction mixture was isolated using preparative LC/MS to provide the desired product as a white powder. 1H NMR (DMSO-d6) δ 8.77 (bs, 1H), 8.45 (bs, 1H), 8.40 (bs, 1H), 8.04 (m, 2H), 7.94 (d, 1H), 7.75 (m, 2H), 7.62 (m, 1H), 6.95 (m, 1H), 6.87 (m, 1H). LC/MS: 380 (M+H)+.

Quelle