Reaktion #5322

Reaktionsgleichung

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

acetic acid

ethyl orthocarbonate

→

Methyl 1-[(2'-cyanobiphenyl-4-yl)methyl]-2-ethoxy-benzimidazole-7-carboxylate

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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

Quelle