反应详情

温度

115 °C

A slurry of anhydrous sodium acetate (60.0 g; 0.73 mol) in acetic acid (400 ml) is stirred and 2-methyl-5-nitrobenzyl chloride (45.3 g; 0.24 mol) added. The resulting reaction mixture is heated to reflux and is heated overnight at 115° C., after which time tlc (silica gel; 75/25 hexane/benzene) indicates that no starting material is present. The mixture is cooled down, concentrated in vacuo, and diluted with water. The precipitated solid (48.9 g; 95.8%) is collected and dried. A sample recrystallized from hexane has a melting point of 52°-53.5° C.

1. customThe resulting reaction mixture
2. temperatureis heated
3. temperatureto reflux
4. temperatureThe mixture is cooled down
5. concentrationconcentrated in vacuo
6. additiondiluted with water
7. customThe precipitated solid (48.9 g; 95.8%) is collected
8. customdried
9. customA sample recrystallized from hexane