反应详情

温度

50 °C

A mixture of 3-amino-2-isopropyl-5-nitrophenol (9.94 g, 47 mmol), K2CO3 (13.00 g, 94 mmol) and toluenesulfonic acid cyanomethyl ester (10.93 g, 52 mmol) in 500 mL DMF was warmed to 50° C. After 16 h the mixture was cooled, poured into 500 mL H2O and extracted with toluene/ethyl acetate (1:1). The combined organics were washed with H2O, washed with brine, filtered and concentrated in vacuo. The crude solid was recrystallized from EtOH to afford (2-isopropyl-4-methoxy-5-nitro-phenoxy)-acetonitrile (8.95 g, 76%) as a yellow crystalline solid.

1. temperatureAfter 16 h the mixture was cooled
2. extractionextracted with toluene/ethyl acetate (1:1)
3. washThe combined organics were washed with H2O
4. washwashed with brine
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude solid was recrystallized from EtOH