Reaktion #974929

Reaktionsgleichung

3-(acetylamino)-6-bromo-2-nitrobenzoic acid

trimethylsilyldiazomethane diethyl ether

→

title compound

Ausbeute 66.4%

methyl 3-(acetylamino)-6-bromo-2-nitrobenzoate

Ausbeute 66.4%

Lösungsmittel

methanol

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   EinengenThe reaction solution was concentrated under reduced pressure
3. 3
   Sonstigethe residue was purified by silica gel column chromatography (ethyl acetate/hexane=25/75→60/40)

Vorschrift

To a mixed solution of 3-(acetylamino)-6-bromo-2-nitrobenzoic acid (2.00 g, 6.60 mmol) in methanol (20 mL) and tetrahydrofuran (5 mL) was added 2M trimethylsilyldiazomethane/diethyl ether solution (10.6 mL, 21.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 5 days. The reaction solution was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=25/75→60/40) to give the title compound (1.39 g, yield 66%).

Quelle