Synthetic method for organically compounding intermediate cyanogen

[0010] Example 1:

[0011] Dissolve 5mol of 1,4-diiodobutane in 5L of 30% acetone solution, control the stirring speed at 110rpm, add 6mol of 4-methyl-benzonitrile, raise the temperature of the solution to 60℃, and reflux for 90min , Reduce the temperature of the solution to 10℃, filter, wash the filter cake with 50% methylamine solution with mass fraction, pour into 20% potassium iodide solution with mass fraction, and the oil layer should be washed with sodium chloride solution, mass fraction is 70% Washing with pentane solution, washing with 80% ethyl acetate solution with mass fraction, 30kPa vacuum distillation, collecting 50°C fractions, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 480.6g of finished oxonitrile with a yield of 89%.

[0012] Example 2:

[0013] Dissolve 5mol of 1,4-diiodobutane in 5L of 32% acetone solution, control the stirring speed to 130rpm, add 6.5mol of 4-methyl-benzonitrile, raise the temperature of the solution to 65℃, and reflux 100min, reduce the temperature of the solution to 12℃, filter, wash the filter cake with a mass fraction of 52% methylamine solution, pour into a 23% potassium iodide solution, and then layer the oil layer with sodium chloride solution, the mass fraction is 72 Wash with %pentane solution, wash with 82% ethyl acetate solution, 35kPa vacuum distillation, collect the 52°C distillate, and dehydrate with anhydrous potassium carbonate dehydrating agent to obtain 491.4g of finished oxonitrile with a yield of 91%.

[0014] Example 3:

[0015] Dissolve 5mol of 1,4-diiodobutane in 5L of 35% acetone solution, control the stirring speed at 150rpm, add 7mol of 4-methyl-benzonitrile, raise the temperature of the solution to 70℃, and reflux for 110min , Reduce the temperature of the solution to 15℃, filter, wash the filter cake with a 55% mass fraction of methylamine solution, pour into a 27% mass fraction of potassium iodide solution, layering occurs, and wash the oil layer with sodium chloride solution, with a mass fraction of 75% Washing with pentane solution, washing with 85% ethyl acetate solution with mass fraction, 40kPa vacuum distillation, collecting 55°C distillate, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 507.6g of finished oxonitrile with a yield of 94%.