Prepn of high-content vitamin E

A vitamin and high-content technology, applied in the direction of organic chemistry, can solve the problems of high cost, complicated process, difficult to meet vitamin E, etc., and achieve the effect of low cost and simple process

Inactive Publication Date: 2006-04-19
ZHEJIANG NHU CO LTD +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But the defective that above-mentioned synthesis method all exists is that intermediate product dl-alpha-tocopherol isomer content is higher, because the boiling point of this isomer is close to vitamin E, make follow-up separation operation (rectification) process complicated, required cost High, and dl-α-tocopherol isomers are difficult to remove, which will easily cause the vitamin E content (purity) of the final product to be slightly lower, generally 93% to 96%
For the vitamin E of medical use, then need content (purity) more than 98% or higher, the vitamin E that makes with above-mentioned various methods is difficult to meet the required content (purity) requirement of medical use

Method used

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  • Prepn of high-content vitamin E
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  • Prepn of high-content vitamin E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: (existing method, promptly do not add procatalyst of the present invention) at room temperature, in the there-necked flask of 500ml, with the zinc chloride of 51.1 grams (331mmol) trimethylhydroquinone and equivalent and 4.7ml Concentrated hydrochloric acid (0.05mmol) was mixed with 150ml ethyl acetate, the solution was heated to 40°C, 100 grams (330mmol) of isophytol was added dropwise within 2 hours, the reaction mixture was kept at 40°C for 1.5 hours, and then the temperature was raised Heat it at 60-65°C for 2 hours, depressurize the reaction solution to recover ethyl acetate, esterify the obtained crude product with acetic anhydride, and then rectify the product to obtain a vitamin E content of 96.0%, dl-α-tocopherol The phenolic isomer content was 2.5%.

Embodiment 2

[0019] Embodiment 2: (the present invention) at room temperature, in the there-necked flask of 500ml, the zinc chloride of 51.1 grams (331mmol) trimethylhydroquinone and equivalent and 4.7ml concentrated hydrochloric acid (0.05mmol) and 150ml ethyl acetate Esters are mixed, add 1.5 grams (being 1.5% of different phytol weight) 1,3,5-trimethoxybenzene, structural formula is

[0020] The amount of isophytol added and the preparation process and process conditions are the same as those in Example 1 to obtain a vitamin E product with a content of 99.3%, and the content of dl-α-tocopherol isomers in the product is 0.29%.

[0021] The difference between Examples 3-10 and Example 2 lies in the cocatalyst added, and the obtained data are listed in Table 1.

[0022] The difference between Examples 11-16 and Example 2 lies in the amount of co-catalyst added, and the obtained data are listed in Table 2. Table 1: select the data table of cocatalyst gain of the present invention for use...

Embodiment 5

[0028] The gas chromatogram data list in embodiment 5 is as follows:

[0029] Peak width (WE)): 3 Slope (SL): 50.00 Calculation method: area normalization method

[0030] Peak No. Component Name Component No. Retention Time Peak Area Peak Height Content Peak Marker

[0031] 1 0 1.21 98.0 56 0.0033 S

[0032] 2 0 1.80 137.8 23 0.0046 S

[0033] 3 0 8.49 90.6 4 0.0030 S

[0034] 4 0 9.07 211.6 13 0.0071 F

[0035] 5 0 9.47 1601.6 82 0.0539 M

[0036] 6 0 9.79 1288.1 51 0.0433 M

[0037] 7 0 10.81 803.1 44 0.0270 M

[0038] 8 0 11.43 2347.3 141 0.0790M

[0039] 9 0 12.39 1243.3 43 0.0418 M

[0040] 10 0 14.03 12373.9 531 0.4162 S

[0041] 11 0 15.15 1284.7 34 0.0432 M

[0042] 12 0 16.27 901.3 28 0.0303 F

[0043] 13 0 18.23 2948150.8 56382 99.1055 M

[0044] 14 0 19.23 1465.8 55 0.0493 M

[0045] 15 0 19.79 1370.8 38 0.0461 M

[0046] 16 0 20.87 47.3 8 0.0016 M

[0047]17 0 21.23 358.8 13 0.0121 M

[0048] 18 0 21.91 152.3 7 0.0051 M

[0049] 19 0 25.07 32.1 1 0...

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Abstract

The present invention relates to the preparation process of high-content vitamin E through condensation of trimethyl hydroquinone and isophytol. In polar ester solvent and in the presence of zinc halide and strong acid, trimethyl hydroquinone and isophytol produce condensation reaction. The present invention features that during condensation reaction, co-catalyst in the amount of 0.1-2.0 wt% of isophytol is added to inhibit the generation of dl-alpha-tocopherol isomer. The present invention can produce vitamin E product with vitamin E content over 98 % for corresponding medicinal use.

Description

technical field [0001] The invention relates to a method for preparing high-content vitamin E by condensation of trimethylhydroquinone and isophytol. Background technique [0002] Vitamin E (dl-alpha-tocopheryl acetate) is a very well-established product that can be produced in a variety of ways. Several existing methods for preparing vitamin E through the condensation reaction of trimethylhydroquinone (also known as trimethylhydroquinone) and isophytol are as follows: [0003] Chemical Abstracts (CA) 103, 104799 (1985), CA 103, 123731 (1985) and CA 110, 39221 (1989), in zinc, zinc chloride and a protic acid such as hydrohalic acid, such as hydrochloric acid, trichloroacetic acid, acetic acid The condensation reaction of trimethylhydroquinone and isophytol is carried out in the presence of other similar acids, especially zinc chloride / hydrochloric acid as a catalyst. [0004] U.S. Patent No. 4,634,781 reported in ZnCl 2 / HCl or a Lewis acid / HCl, e.g., boron trifluoride (B...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/72
Inventor 陈晓阳陈富场
Owner ZHEJIANG NHU CO LTD
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