6-氯-2,3-二氟苯腈

反应条件: temp:190.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 24.8 g (0.135 mol) of 2,3-difluoro-6-nitrobenzonitrile and 1 g of anhydrous calcium chloride are placed in a 50 ml flask with a finely drawn-out gas inlet tube, and heated to 190° C. Chlorine is introduced at this temperature with a throughput of 2-3 l/h so that a uniform production of nitrous gases occurs. After a reaction time of 12 h, the starting material has been substantially converted (<10% residual content of nitro compound). The remaining nitrous gases are purged with air and the residue is distilled off under vacuum over a short Vigreux column to give 15.5 g (89 mmol, 66%) of 2-chloro-5,6-difluorobenzonitrile as a light yellowish, oily liquid boiling at 70°-75° C./3 Torr (purity (GC)>95%). After a reaction time of 12 h The remaining nitrous gases are purged with air the residue is distilled off under vacuum over a short Vigreux column

反应条件: temp:190.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 24.8 g (0.135 mol) of 2,3-difluoro-6-nitrobenzonitrile and 1 g of anhydrous calcium chloride are placed in a 50 ml flask with a finely drawn-out gas inlet tube, and heated to 190° C. Chlorine is introduced at this temperature with a throughput of 2-3 l/h so that a uniform production of nitrous gases occurs. After a reaction time of 12 h, the starting material has been substantially converted (<10% residual content of nitro compound). The remaining nitrous gases are purged with air and the residue is distilled off under vacuum over a short Vigreux column to give 15.5 g (89 mmol, 66%) of 2-chloro-5,6-difluorobenzonitrile as a light yellowish, oily liquid boiling at 70°-75° C./3 Torr (purity (GC)>95%). After a reaction time of 12 h The remaining nitrous gases are purged with air the residue is distilled off under vacuum over a short Vigreux column

反应条件: temp:190.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 24.8 g (0.135 mol) of 2,3-difluoro-6-nitrobenzonitrile and 1 g of anhydrous calcium chloride are placed in a 50 ml flask with a finely drawn-out gas inlet tube, and heated to 190° C. Chlorine is introduced at this temperature with a throughput of 2-3 l/h so that a uniform production of nitrous gases occurs. After a reaction time of 12 h, the starting material has been substantially converted (<10% residual content of nitro compound). The remaining nitrous gases are purged with air and the residue is distilled off under vacuum over a short Vigreux column to give 15.5 g (89 mmol, 66%) of 2-chloro-5,6-difluorobenzonitrile as a light yellowish, oily liquid boiling at 70°-75° C./3 Torr (purity (GC)>95%). After a reaction time of 12 h The remaining nitrous gases are purged with air the residue is distilled off under vacuum over a short Vigreux column