反应详情

温度

64 °C

To a jacketed reactor, acetic acid (450 mL) and acetic anhydride (225 mL) is charged at 10° C. Then, to the above mixture, NalO4 powder (97.2 g) and Iodine (77.2 g) is added under stirring. While keep internal temperature at below 30° C., conc. H2SO4 (720 mL) is added dropwise. Then, 2-chloro-nitrobenzene (Rt=11.11 min) is added in one portion, and heat the mixture gradually to 64° C. The resulting mixture continues to be stirred for usually at least 2 hours until process monitor shows almost complete conversion. Then, the mixture is cooled down to room temperature, and transferred slowly into another jacketed reactor with pre-cooled cold Na2SO3 solution (250 g Na2SO3 in 2000 mL water). Collect the wet cake by filtration and wash the cake with water (450 mL×2), then purification of the cake with n-heptane crystallization to afford 2-chloro-5-iodonitrobenzene in 62% yield and 98% HPLC purity (Rt=15.75 min).

1. customat below 30° C.
2. stirringto be stirred for usually at least 2 hours until process monitor
3. temperatureThen, the mixture is cooled down to room temperature
4. customtransferred slowly into another jacketed reactor
5. customCollect the wet cake
6. filtrationby filtration
7. washwash the cake with water (450 mL×2)
8. custompurification of the cake
9. customwith n-heptane crystallization