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Synthetic method of 1,2,4-butanetriol

A synthesis method and diol technology are applied in alcoholysis preparation, organic chemistry and other directions, which can solve the problems of unstable yield and difficult post-processing, and achieve the effects of low price, easy operation and improved yield.

Active Publication Date: 2013-03-13
内蒙古佳瑞米精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The present invention provides an optimized synthetic method of 1,2,4-butanetriol, which overcomes the problems of unstable yield and difficult post-processing in previous synthetic routes

Method used

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  • Synthetic method of 1,2,4-butanetriol

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The 1.0L two-necked bottle is equipped with electromagnetic stirring, thermometer, water separator and condenser. 352.0 g of 1,4-but-2-enol, 126.3 g of paraformaldehyde, 1.6 g of p-toluenesulfonic acid, 48.1 g of 4,6-dinitro-2-sec-butylphenol, and 263.0 g of cyclohexane were added. After reflux for 16 hours, 83.1 g of water was separated. Take the vacuum distillation device instead. Under 12KPa, the fraction between 40°C and 56°C was collected, and a total of 372.5g of the product was obtained, with a normalized content of 96.98% and a yield of 90.21%.

Embodiment 2

[0033] 17.7g of 1,4-but-2-enol, 6.3g of paraformaldehyde, 0.1g of p-toluenesulfonic acid, 0.5g of 4,6-dinitro-2-sec-butylphenol, dissolved in 13.2g of cyclohexane . After reflux for 16 hours, 4.1 g of water were separated. Take the vacuum distillation device instead. Under 12KPa, the fraction between 40°C and 56°C was collected to obtain a total of 17.1g of the product, with a normalized content of 95.99% and a yield of 81.97%.

Embodiment 3

[0035]17.7g of 1,4-but-2-enol, 6.3g of paraformaldehyde, 0.1g of p-toluenesulfonic acid, 4.8g of 4,6-dinitro-2-sec-butylphenol, dissolved in 13.2g of cyclohexane . After reflux for 16 hours, 4.3 g of water were separated. Take the vacuum distillation device instead. Under 12KPa, the fraction between 40°C and 56°C was collected to obtain a total of 18.8g of the product, with a normalized content of 96.59% and a yield of 90.77%.

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Abstract

The invention discloses a synthetic method of 1,2,4-butanetriol, which belongs to the field of organic chemistry. The synthetic method comprises the following steps: firstly, carrying out condensation on 2-butene-1,4-diol and paraformaldehyde under the catalysis of p-toluenesulfonic acid, and reacting the obtained condensation product 2 with H2O2 under the catalysis of Na2HPO4 so as to generate an epoxy compound 3, wherein through addition of an appropriate inhibitor, the yields of the compounds 2 and 3 are improved; and then, carrying out catalytic hydrogenation on the epoxy compound 3 in the presence of Raney Ni-4 so as to obtain a compound 4, and carrying out esterification and ring opening on the compound 4, then carrying out acid catalytic transesterification to obtain 1,2,4-butanetriol. The synthetic method disclosed by the invention is more stable and reliable, and easy to operate; used reagents are low in cost and process conditions are mild; and butanetriol with an external standard content being more than 95% can be obtained just through simple refining.

Description

technical field [0001] The invention relates to a synthesis method of 1,2,4-butanetriol, which belongs to the field of organic chemistry. Background technique [0002] 1,2,4-Butanetriol is an important chemical intermediate in organic synthesis, widely used in the fields of military industry, medicine, tobacco, cosmetics, papermaking, agriculture and polymer materials. Its nitro compound is a good energetic plasticizer, which can replace nitroglycerin as NEPE propellant and high-energy, high-tech propellant; in medicine, it can be used as a drug slow-release agent to control the release rate of the drug; as a tobacco additive, It can eliminate the poison of nitro compounds to the human body and reduce the damage of tar components; as an important antimicrobial component, it can effectively prevent the growth of microorganisms; it can increase the color and adhesion in the color developer; in the field of polymer materials , can be used as a cross-linking agent for polymer m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/22C07C29/128
Inventor 杜志博秦学孔
Owner 内蒙古佳瑞米精细化工有限公司