Method for preparing 2-ethylhexyl chloroformate

A technology of ethylhexyl and chloroformic acid, which is applied in the preparation of 2-ethylhexyl chloroformate and the field of preparation of 2-ethylhexyl chloroformate, can solve the problem of unfavorable 2-ethylhexyl chloroformate Ester synthesis, storage, transportation, dangerous operation, difficult control and operation of liquid phosgene, etc., to achieve the effect of low toxicity, convenient weighing and mild reaction conditions

Inactive Publication Date: 2009-12-16
ZHENGZHOU UNIV
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  • Abstract
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Problems solved by technology

However, because liquid phosgene is difficult to control and operate in the production process, there are many unsafe factors, and it is difficult to carry out industrial production
Wang Chaohui and Yang Weiguo (pilot test research on the production technology of 2-ethylhexyl chloroformate. Sichuan Chemical Industry, 2008, (3): 36) studied the synthesis technology of 2-ethylhexyl chloroformate, and pointed out that if the raw material phosgene Containing a certain amount of water in the isooctanol is unfavorable for the synthesis of 2-ethylhexyl chloroformate, and at the same time, the non-volatile organic impurities in the raw materials will affect the appearance quality of EHP
[0005] The current related research has not yet solved the problem of the purity of phosgene, and phosgene cannot be accurately measured in the reaction process, and it is difficult to perform an equivalence ratio reaction.
At the same time, the toxicity of phosgene puts forward higher requirements on equipment, and its storage, transportation, and operation are still quite dangerous, which brings a series of difficulties to industrial production.

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  • Method for preparing 2-ethylhexyl chloroformate
  • Method for preparing 2-ethylhexyl chloroformate

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Experimental program
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Effect test

Embodiment 1

[0019] Solid phosgene (77g), sodium carbonate (55g), and catalyst N,N-dimethylformamide (10g) were mixed uniformly, and stirred in toluene (750mL) at 0°C for 30 minutes. Then, 750 mL of 2-ethylhexanol / toluene solution with a concentration of 0.69 mol / L was slowly dropped into the mixture for 30 minutes. After the reaction system was stirred at 0° C. for 8 hours, sodium carbonate was separated by suction filtration, and then the solvent was separated by distillation under reduced pressure to obtain 89 g of a colorless oily liquid, namely 2-ethylhexyl chloroformate, with a yield of 93.2%. The purity of 2-ethylhexyl chloroformate obtained by titration analysis was 98%.

[0020] The proton nuclear magnetic spectrum of product 2-ethylhexyl chloroformate is as figure 1 , the chemical shift of the chemical environment of the hydrogen on 2-ethylhexyl chloroformate is located at δ0.93[6H, CH 3 (1)], 1.33 [6H, CH 2 (2)], 1.41 [2H, CH 2 (3)], 1.65[1H, CH(4)], 4.2[2H, CH 2 (5)]. The...

Embodiment 2

[0022] Solid phosgene (77g), anhydrous sodium bicarbonate (44g), and catalyst triethylamine (13.1g) were mixed uniformly, and stirred in dichloromethane (750mL) at 0°C for 30 minutes. Then, 750 mL of 2-ethylhexanol / dichloromethane solution with a concentration of 0.69 mol / L was slowly dropped into the mixture for 30 minutes. After the reaction system was stirred at 0°C for 8 hours, sodium bicarbonate was separated by suction filtration, and then the solvent was separated by distillation under reduced pressure to obtain 87 g of a colorless oily liquid, namely 2-ethylhexyl chloroformate, with a yield of 91.1%. , the purity obtained by titration analysis of 2-ethylhexyl chloroformate is 98%.

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Abstract

The invention relates to a method for preparing 2-ethylhexyl chloroformate, which belongs to the technical field of organic chemical synthesis. The method comprises the steps of: evenly mixing solid phosgene, a catalyst, and alkaline substance (carbonate or hydrocarbonate) in an organic solvent according to a certain molar ratio; stirring the mixture for 10 to 30 minutes at a temperature of between 5 DEG C below zero and 25 DEG C; adding 2-ethylhexanol diluted by the organic solvent into the mixture; reacting for 1 to 48 hours at a temperature of between 5 DEG C below zero and 25 DEG C; and obtaining the 2-ethylhexyl chloroformate through suction filtration and reduced pressure distillation. The method has the advantages of simple process method, mild reaction conditions, and replacement of the phosgene by the solid phosgene as a raw material; the solid phosgene has safe use, is environment-friendly, has accurate metering, and is convenient to store and transport, and the synthesized 2-ethylhexyl chloroformate has higher yield and purity. The method is applicable to the industrialized production of the 2-ethylhexyl chloroformate further to synthesize an initiator, namely bis-(2-ethylhexyl)peroxydicarbonate (EHP).

Description

technical field [0001] The invention relates to a preparation method of 2-ethylhexyl chloroformate, in particular to a method for preparing high-yield 2-ethylhexyl chloroformate by substituting solid phosgene for phosgene, and belongs to the technical field of organic chemical synthesis. Background technique [0002] Alkyl chloroformate R-OCOC1 can be used to prepare intermediates of pesticides, perfumes, pigments, drugs, polymers and other chemicals. The reaction between chloroformate and various sulfonates is used to identify ores, and chloroformate can also be used to prepare polyurethane and foam latex, which are raw materials for optical lenses. Some of the chloroesters can also be used as inhibitors of amines, and many heterocyclic compounds can be synthesized. [0003] 2-Ethylhexyl chloroformate can be used to synthesize bis(2-ethyl)hexyl peroxydicarbonate (abbreviated as EHP), which is a colorless and transparent liquid, and EHP is a highly active initiator. Compar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08B01J31/02
Inventor 赵清香刘民英付鹏王玉东才勇
Owner ZHENGZHOU UNIV
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