Réaction #699952

Équation de réaction

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

methyl chloroformate

→

needles

Rendement 90.0%

Methyl 2-[(2'-cyanobiphenyl-4-yl)methylamino]-3-methoxycarbonylaminobenzoate

Rendement 90.0%

Solvants

pyridine

Conditions de réaction

Traitement

1. 1
   Températurecooling
2. 2
   Concentrationconcentrated
3. 3
   ExtractionThe residue was extracted with ethyl acetate
4. 4
   LavageThe extract was washed with water
5. 5
   Autredried
6. 6
   Autreevaporated
7. 7
   AutreThe residue was recrystallized from ethyl acetate

Mode opératoire

To a stirred solution of methyl 3-amino-2-[(2'-cyanobiphenyl-4-yl)methylamino]benzoate (10 g) in pyridine (50 ml) was added dropwise methyl chloroformate (9.0 ml) under ice-cooling. The mixture was stirred at room temperature for 3 hours and concentrated. The residue was extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was recrystallized from ethyl acetate--hexane to afford pale yellow needles (10.5 g, 90%), m.p. 113-115° C.

Source