反应详情

Sodium iodide (229.2 g) was added to a solution of 4-chloromethyl benzoic acid tert-butyl ester (315.2 g) in acetone (1.5 L). The reaction mixture was heated to reflux for about 2 h and then allowed to cool to room temperature. The precipitate was removed by filtration and the filtrate concentrated under reduced pressure. The residue was partitioned between water (500 mL) and MTBE (1500 mL). The organic phase was washed with saturated sodium bicarbonate and dried over magnesium sulfate. Concentration under reduced pressure afforded 442.2 g (97% yield) dark oil. HNMR: CDCl3, 1.59 ppm (s, 9H), 4.47 (s, 2H), 7.42 (d, 2H), 7.91 (d, 2H)

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for about 2 h
3. customThe precipitate was removed by filtration
4. concentrationthe filtrate concentrated under reduced pressure
5. customThe residue was partitioned between water (500 mL) and MTBE (1500 mL)
6. washThe organic phase was washed with saturated sodium bicarbonate
7. dry with materialdried over magnesium sulfate
8. concentrationConcentration under reduced pressure