Chemical synthesis method of 3,4-dichlorobenzene isocyanate
A technology for chemical synthesis of dichlorobenzene isocyanate, applied in the fields of pesticides, dyes, and synthetic medicines, can solve the problems of serious equipment corrosion, long reaction period, and large safety hazards, and achieves small equipment corrosion, low production cost, and safe and reliable production. Effect
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Embodiment 1
[0013] 3,4-dichloroaniline: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1:0.35:0.01 (molar ratio), the amount of toluene is 3,4-di 10 times the mass of chloroaniline.
[0014] First, add 3,4-dichloroaniline, 1,3-dimethyl-2-imidazolidinone and toluene into the reaction kettle, start stirring, after stirring evenly, add bis(trichlorohydrin) dropwise within 1 hour at room temperature Toluene solution of methyl)carbonate, and then heated up and refluxed for 4 hours. After the reaction, the toluene was recovered by distillation under reduced pressure. Finally, the fraction at 120-122°C was collected at 2.6Kpa, solidified after cooling, with a melting point of 42-43°C and a content of 99.2 %, yield 95.2%.
Embodiment 2
[0016] 3,4-dichloroaniline: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1:0.35:0.005 (molar ratio), the amount of reclaimed toluene is 3,4- 10 times the mass of dichloroaniline. According to the operation of Example 1, the final product obtained has a melting point of 42-43° C., a content of 99.5%, and a yield of 96.0%.
Embodiment 3
[0018] 3,4-dichloroaniline: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1:0.5:0.01 (molar ratio), the amount of toluene is 3,4-di 10 times the mass of chloroaniline.
[0019] According to the operation of Example 1, the final product has a melting point of 41-43° C., a content of 99.0%, and a yield of 96.5%.
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