반응 #72516

반응 방정식

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

수율 70.2%

용매

ethyl acetate

sulfolane

반응 조건

후처리

1. 1
   세척washed with water (5×50 mL)
2. 2
   농축The organic layer (aqueous emulsion) was concentrated
3. 3
   기타to give an aqueous slurry which
4. 4
   여과was filtered
5. 5
   세척washed with water (50 mL)
6. 6
   기타The product was dried under high vacuum at 60° C.

실험 절차

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.

출처