Reaktion #5335

Reaktionsgleichung

water

methyl 2-(N-tert-butoxycarbonylamino)-3-nitrobenzoate

4'-bromomethylbiphenyl-2-carboxamide

K2CO3

→

syrup

Ausbeute 90.0%

Methyl 2-[N-tert-butoxycarbonyl-N-(2'-carbamoylbiphenyl-4-yl)methylamino1-3-nitrobenzoate

Ausbeute 90.0%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated for 6 hours
2. 2
   Temperaturunder reflux
3. 3
   Extraktionthe mixture was extracted with ethyl acetate
4. 4
   WaschenThe extract was washed with water
5. 5
   Trocknendried over MgSO4
6. 6
   SonstigeThe solvent was removed in vacuo
7. 7
   Sonstigethe residue was purified by column chromatography on silica gel

Vorschrift

A mixture of methyl 2-(N-tert-butoxycarbonylamino)-3-nitrobenzoate (1.8 g), 4'-bromomethylbiphenyl-2-carboxamide (1.8 g) and K2CO3 (0.86 g) in acetonitrile (25 ml) was heated for 6 hours under reflux. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over MgSO4. The solvent was removed in vacuo, and the residue was purified by column chromatography on silica gel to afford a yellow syrup (2.3 g, 90%).

Quelle