反应详情

To a mixture of 4-nitrophenol (200 grm, 1.439 mol), anhydrous K2CO3 (800 grm, 5.789 mol) and sodium iodide (10 g, 66.7 mmol) in anhydrous acetone (2.75 L) was added methyl 2-chloropropionate (264 g, 2.154 mol) and refluxed for 20 hours. Acetone was distilled off and water (3 L) was added. Crude 14 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 14 (100 g, 31%) as a white fluffy powder with a m.p between 83-84° C.

1. temperaturerefluxed for 20 hours
2. distillationAcetone was distilled off
3. additionwater (3 L) was added
4. filtrationCrude 14 was filtered
5. customdried
6. customrecrystallised from a mixture of ethyl acetate:hexane (1:5)