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Aminomethylation method for tocopherol concentrated solution

A technology of amine methylation and tocopherol, which is applied in the field of amine methylation of tocopherol concentrate, can solve the problems of complex process, hindering production progress, low yield, etc., and achieve stable products, stable production technology, The effect of mild reaction

Inactive Publication Date: 2012-07-18
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity of the process and low yield, it is currently the bottleneck hindering production progress

Method used

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  • Aminomethylation method for tocopherol concentrated solution
  • Aminomethylation method for tocopherol concentrated solution
  • Aminomethylation method for tocopherol concentrated solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] All instruments and equipment are laboratory-scale. The content of mixed tocopherols in the raw tocopherol concentrate is 36.30%, of which α-tocopherol accounts for 8.09%, β, γ-tocopherol accounts for 63.03%, and δ-tocopherol accounts for 28.88%.

[0031] Take 75g of tocopherol concentrate (about 0.06mol of non-α-tocopherol) in the reactor, add 21.6g (about 0.19mol) of dimethylamine aqueous solution (40%), then add 106mL of toluene solvent, and open it after purging three times with nitrogen Stir, control the temperature below 35°C, slowly add 16.5g (about 0.20mol) formaldehyde aqueous solution (37%) into the reactor dropwise within 20min, then raise the temperature to 90°C, condense and reflux for 2.5h to stop the reaction; Liquid separator, after standing for 0.5h, drain the lower water phase and the impurities in the interlayer, transfer the mother liquor to the desolventizer; finally raise the temperature to 120°C to distill the toluene out, stop the reaction when th...

Embodiment 2

[0036] Take 75g of tocopherol concentrate (about 0.06mol of non-α-tocopherol) in the reactor, add 21.6g (about 0.19mol) of dimethylamine aqueous solution (40%), then add 106ml of cyclohexane solvent, and blow nitrogen three times Then start stirring, control the temperature below 35°C, slowly add 16.5g (about 0.20mol) formaldehyde aqueous solution (37%) into the reactor dropwise within 20min, then raise the temperature to 80°C, condense and reflux for 2.5h and then stop the reaction; The liquid was transferred into the liquid separator, and after standing for 0.5h, the impurities in the lower aqueous phase and the interlayer were discharged, and the mother liquor was transferred to the desolventizer; finally, the temperature was raised to 90°C to distill the cyclohexane, and the reaction was stopped when there was no distillate. , cooling, sampling and weighing, the product is a mixture of impurities other than α-tocopheryl alkaloids and glycerides.

[0037] Take 2-3 drops of ...

Embodiment 3

[0041] Take 75g of tocopherol concentrate (about 0.06mol of non-α-tocopherol) in the reactor, add 36.5g (about 0.20mol) of diethylamine aqueous solution (40%), then add 110ml of cyclohexane solvent, and blow nitrogen three times Then start stirring, control the temperature below 35°C, slowly add 16.5g (about 0.20mol) formaldehyde aqueous solution (37%) into the reactor dropwise within 20min, then raise the temperature to 85°C, condense and reflux for 4.5h to stop the reaction; The liquid was transferred into the liquid separator, and after standing for 0.5h, the impurities in the lower aqueous phase and the interlayer were discharged, and the mother liquor was transferred to the desolventizer; finally, the temperature was raised to 90°C to distill the cyclohexane, and the reaction was stopped when there was no distillate. , cooling, sampling and weighing, the product is a mixture of impurities other than α-tocopheryl alkaloids and glycerides.

[0042] Take 2-3 drops of the pre...

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Abstract

The invention discloses an aminomethylation method for a tocopherol concentrated solution, which belongs to the field of fine organic synthesis. The tocopherol concentrated solution is a product prepared by distilling and purifying a plant oil deodorized distillate, and contains high-content mixed tocopherols (alpha, beta, gamma and delta-tocopherols). The beta, gamma and the delta-tocopherols are called non-alpha-tocopherol. A Mannic reaction is a condensation process of three components, i.e., a Mannich alkali serving as a product is prepared by condensing amine, aldehyde and non-alpha-tocopherol containing active hydrogen. In the invention, a high-yield Mannich alkali, i.e., non-alpha-tocopherol is generated by adopting a 'one-pot method', adding an amine reagent, an aldehyde reagent and the tocopherol concentrated solution into a reaction system and undergoing an aminomethylation reaction in the presence of an organic solvent. Due to the adoption of the method, the convention rate of the non-alpha-tocopherol can be over 99 percent in the absence of a catalyst, and the yield of the non-alpha-tocopherol generated in the reaction is over 98 percent.

Description

technical field [0001] The invention discloses an amino methylation method for a concentrated tocopherol solution. The preparation method achieves the purpose of increasing the yield of a target product, and belongs to the field of fine organic synthesis. Background technique [0002] Vitamin E, also known as tocopherol, has two types: synthetic and natural. Natural vitamin E is a mixture of four tocopherols and four tocopherol trienols, which is optically active; chemical synthetic products usually refer to DL-α-tocopherol, which is a racemic form of various optical isomers. body. Because natural vitamin E is superior to chemical synthetic products in terms of biological activity and safety, people tend to use natural vitamin E in medicine, food, cosmetics and feed additives. Therefore the present invention focuses on the development and utilization of research natural vitamin E. Tocopherol concentrate is a product purified from deodorized vegetable oil distillates throu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
Inventor 蒋平平李海洋董玉明印建国
Owner JIANGNAN UNIV
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