Reaktion #484290

Reaktionsgleichung

Acetic acid

methyl 3-amino-2-[[(2′-cyanobiphenyl-4-yl)methyl]amino]benzoate

ethyl orthocarbonate

→

Methyl 1-[(2′-cyanobiphenyl-4-yl)methyl]-2-ethoxybenzimidazole-7-carboxylate

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated to dryness
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   WaschenThe solution was washed with an aqueous solution of sodium hydrogen carbonate and water
4. 4
   SonstigeThe solvent was evaporated in vacuo
5. 5
   Sonstigeto give crystals
6. 6
   SonstigeRecrystallization from ethyl acetate-hexane afforded colorless crystals (2.01 g, 86%), m.p. 168.5-169.5° C.

Vorschrift

Acetic acid (0.37 g) was added to a solution of methyl 3-amino-2-[[(2′-cyanobiphenyl-4-yl)methyl]amino]benzoate (2.03 g) in ethyl orthocarbonate (5 ml), and the mixture was stirred at 80° C. for one hour. The reaction mixture was concentrated to dryness and the residue was dissolved in ethyl acetate. The solution was washed with an aqueous solution of sodium hydrogen carbonate and water. The solvent was evaporated in vacuo to give crystals. Recrystallization from ethyl acetate-hexane afforded colorless crystals (2.01 g, 86%), m.p. 168.5-169.5° C.

Quelle