반응 #45798

반응 방정식

5-Bromo-4-fluoro-2-hydroxy-3-nitrobenzoic acid

potassium carbonate

dimethyl sulfate

→

compound

수율 92.0%

Methyl 5-bromo-4-fluoro-2-methoxy-3-nitrobenzoate

수율 92.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타the insoluble matter was removed by filtration (with washing with acetonitrile (400 ml))
2. 2
   농축The filtrate was concentrated under reduced pressure (about 800 ml of acetonitrile
3. 3
   기타was evaporated away), and water (800 ml)
4. 4
   workup.ADDITIONwas added to the residue
5. 5
   세척The precipitated crystal was washed with water
6. 6
   기타dried

실험 절차

5-Bromo-4-fluoro-2-hydroxy-3-nitrobenzoic acid (I-228) (35.89 g, 0.128 mol) was dissolved in acetonitrile (600 ml), then at room temperature, potassium carbonate (53.1 g, 0.358 mol) was added, and dimethyl sulfate (30.3 ml, 0.32 mol was dropwise added. After staring at 60° C. for 2.5 hour and then cooling to room temperature, the insoluble matter was removed by filtration (with washing with acetonitrile (400 ml)). The filtrate was concentrated under reduced pressure (about 800 ml of acetonitrile was evaporated away), and water (800 ml) was added to the residue, followed by stirring at room temperature. The precipitated crystal was washed with water and dried to obtain the entitled compound (36.5 g, 92%) as a pale yellow solid.

출처