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Method for synthesizing N, N'-diisopropylcarbodiimide by using oxygen as oxidant

A technology of diisopropylcarbodiimide and diisopropylthiourea, which is applied in the field of organic chemical synthesis, can solve problems such as large amount of waste brine and difficult to handle, achieves reduction of environmental protection investment, environmental protection of process steps, and improved reaction Yield effect

Inactive Publication Date: 2020-12-29
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for synthesizing N,N'diisopropylcarbodiimide using oxygen as an oxidant, the process steps are safe and reliable, the reaction yield and product purity are high, and it solves the problem of the large amount of waste brine in the traditional process. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add N,N'diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.5:1, add MoO 3 Catalyst, the amount of MoO3 catalyst is 2% of the total material amount (that is, the total mass of N,N'diisopropylthiourea and xylene), and the mass of N,N'diisopropylthiourea and oxygen The ratio is 1:0.3, and the temperature is raised to 120°C for 3.5 hours under the pressure of 10MPa to carry out the oxidation reaction, and then the temperature is lowered to 5°C for suction filtration, and DIC is obtained by decolorization and vacuum distillation. The yield is 94.50%, and the purity is 99.55%. The waste water produced by oxidation can be recycled after passing the test after distillation.

Embodiment 2

[0027] Add N,N'diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.6:1, add MoO 3 Or Sb2O4 catalyst, the amount of MoO3 or Sb2O4 catalyst is 3% of the total material amount, and oxygen is introduced, the mass ratio of N,N'diisopropylthiourea and oxygen is 1:0.4, and the temperature is raised to 110°C under 5MPa pressure Oxidation reaction was carried out for 3h, and then the temperature was lowered to 10°C for suction filtration, and DIC was obtained by decolorization and vacuum distillation. The yield is 94.00%, and the purity is 99.50%. The waste water produced by oxidation can be recycled after passing the test after distillation.

Embodiment 3

[0029] Add N,N'diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 2:1, add Sb 2 O4 catalyst, the amount of Sb2O4 catalyst is 1% of the total material amount, oxygen is introduced, the mass ratio of N,N'diisopropylthiourea and oxygen is 1:0.2, and the temperature is raised to 115°C under 8MPa pressure for oxidation reaction 4h, then cooled to 15°C and filtered with suction, decolorized and distilled under reduced pressure to obtain DIC. The yield is 94.55%, and the purity is 99.55%. The waste water produced by oxidation can be recycled after passing the test after distillation.

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PUM

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Abstract

The invention relates to a method for synthesizing N, N'-diisopropylcarbodiimide by using oxygen as an oxidant, which comprises the following steps: adding N, N'-diisopropylthiourea and a xylene solvent into a high-pressure reaction kettle in a mass ratio of 1-2:1; adding a MoO3 or Sb2O4 catalyst, wherein the use amount of the MoO3 or Sb2O4 catalyst is 1-3% of the amount of the added materials; introducing oxygen, wherein the mass ratio of the N, N'-diisopropylthiourea to the oxygen is 1:0.2-0.4, and an oxidation reaction is carried out for 3-4 h under the conditions that the pressure is controlled to be 5-10 MPa and the temperature is controlled to be 110-120 DEG C; and cooling to 5-15 DEG C, carrying out suction filtration, decolorizing, and carrying out reduced pressure distillation toobtain the DIC. Oxygen is used as an oxidizing agent, the reaction selectivity is high, the risk is low, meanwhile, the wastewater yield is greatly reduced, treatment is easy, and the problem that waste brine in a traditional process is large in amount and difficult to treat is solved; and the method is easy to control, the reaction yield is increased, and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant. Background technique [0002] N,N'-diisopropylcarbodiimide (DIC) is a good low-temperature biochemical dehydrating agent, used for the synthesis and dehydration of amikacin and amino acids, and also used for acids, anhydrides, aldehydes, ketones, etc. The synthesis of this product is also used in the synthesis of peptides and nucleic acids. Used as a dehydrating agent or carboxyl activator for polypeptide synthesis, or for coupling small molecular compounds and polypeptides to carrier proteins. In recent years, the sales situation of DIC has continued to grow, and the supply of products is in short supply. At the same time, the pressure of environmental protection is high, and wastewater treatment has become a difficult problem today. [0003] At present, there are three main m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
CPCC07C267/00
Inventor 张永霞李保铃姜福元殷福东王亮亮方志康
Owner SHANDONG HUIHAI PHARMA & CHEM
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