反应详情

o-Nitrophenol (111.2 g., 0.8 mole), 1-bromopropane (98.4 g., 0.8 mole), anhydrous potassium carbonate (121.4 g., 0.88 mole) and any acetone (800 cc) are refluxed for 70 hrs., filtered the reaction mass, the residue was washed with acetone, and the filtrate rotoevaporated. To the residue of the evaporation was added 200 cc of dichloromethane and rotoevaporated again; the residue was washed with 100 cc of water and separated into two layers. The dichloromethane layer was washed with 100 cc of 10% Na2CO3, separated again, washed again with 100 cc of water, and the dichloromethane layer was fractionated under vacuum. The main fraction distilled at 103°-106° C. at 0.2-0.3 mm Hg., giving 130 g. of product (87% yield).

1. filtration, filtered the reaction mass
2. washthe residue was washed with acetone
3. customTo the residue of the evaporation
4. additionwas added 200 cc of dichloromethane
5. washthe residue was washed with 100 cc of water
6. customseparated into two layers
7. washThe dichloromethane layer was washed with 100 cc of 10% Na2CO3
8. customseparated again
9. washwashed again with 100 cc of water
10. distillationThe main fraction distilled at 103°-106° C. at 0.2-0.3 mm Hg
11. custom, giving 130 g