Reaktion #72516

Reaktionsgleichung

2-amino-N-(2-chloropyridin-3-yl)-5-methylbenzamide

hydrogen chloride

→

8-methyl-5H-benzo[e]pyrido[3,2-b][1,4]diazepin-6(11H)-one

Ausbeute 70.2%

Lösungsmittel

ethyl acetate

sulfolane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with water (5×50 mL)
2. 2
   EinengenThe organic layer (aqueous emulsion) was concentrated
3. 3
   Sonstigeto give an aqueous slurry which
4. 4
   Filtrationwas filtered
5. 5
   Waschenwashed with water (50 mL)
6. 6
   SonstigeThe product was dried under high vacuum at 60° C.

Vorschrift

A solution of 2-amino-N-(2-chloropyridin-3-yl)-5-methylbenzamide (2.515 g, 9.61 mmol) in sulfolane (15 mL) was treated with hydrogen chloride (0.25 mL, 1.0 mmol; 4N in dioxane). The reaction mixture was heated to 220° C. under microwave conditions for 8 minutes. The reaction mixture was then diluted with ethyl acetate (75 mL) and washed with water (5×50 mL). The organic layer (aqueous emulsion) was concentrated to give an aqueous slurry which was filtered and washed with water (50 mL). The product was dried under high vacuum at 60° C. to afford 8-methyl-5H-benzo[e]pyrido[3,2-b][1,4]diazepin-6(11H)-one (1.52 g) that was used without further purification. LCMS [M+H]: 226.

Quelle