反应详情

温度

10 °C

This compound is synthesized according to Makosza, et al with some modifications (Makosza, M., et al, Tetrahedron (1974), 30: 3723). A solution of 4-chloronitrobenzene (31.5 g, 0.2 mol) in pyridine (100 mL) is added dropwise to a vigorously stirred suspension of KOH (fine powder 70.0 g) and α-methylbenzylcyanide (26.2 g, 0.2 mol) in pyridine (150 mL), with the reaction temperature being maintained at 10° C. The reaction mixture is stirred for 24 hours at 25° C., and poured onto an excess of HCl-ice mixture. The acidic aqueous mixture is extracted with benzene, the organic phase washed with brine, dried (Na2SO4), and the benzene evaporated under vacuum. A crude product 42.5 g (84 wt %) results and is recrystallized from isopropanol-petroleum ether to give Compound 7 as white crystals,

1. customThis compound is synthesized
2. extractionThe acidic aqueous mixture is extracted with benzene
3. washthe organic phase washed with brine
4. dry with materialdried (Na2SO4)
5. customthe benzene evaporated under vacuum
6. customA crude product 42.5 g (84 wt %) results
7. customis recrystallized from isopropanol-petroleum ether