Réaction #5322

Équation de réaction

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

Conditions de réaction

Traitement

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

Mode opératoire

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%).

Source