반응 #5322

반응 방정식

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

반응 조건

후처리

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

실험 절차

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%).

출처