Réaction #364649

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—hexane

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