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Method for cleaner production of vitamin A intermediate product

A clean production and vitamin technology, applied in the field of pharmaceutical biochemical industry, can solve the problems of low conversion rate, long reaction cycle, environmental pollution and hidden dangers of operation safety, etc., and achieve the effect of high conversion rate, short production process and convenient industrial production

Active Publication Date: 2015-03-11
XINFA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Aiming at the problems of long reaction cycle, low conversion rate, environmental pollution and operational safety hazards in the prior art, which are not conducive to industrial production, the present invention provides a key intermediate of vitamin A that is clean, environmentally friendly, has a short process, is safe to operate, and is low in cost Clean production method, that is, a preparation method for tetraethyl methylene diphosphonate and tetramethyl methylene diphosphonate for industrial production

Method used

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  • Method for cleaner production of vitamin A intermediate product
  • Method for cleaner production of vitamin A intermediate product
  • Method for cleaner production of vitamin A intermediate product

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Add 276 grams of diethyl phosphite, 114 grams of diethoxymethane, 50 grams of absolute ethanol, and 2 grams of p-toluene sulfonic acid to a dry 1000 ml glass flask, and the temperature is raised to 75-80°C for 5 hours. GC detects that the phosphite diester reaction is complete, cool to 20°C, add 5 g of 28wt% sodium ethoxide ethanol solution to neutralize, distill at 180°C in a vacuum oil bath, collect the 130-136°C / 12 mbar fraction to obtain methylene 265 grams of tetraethyl bisphosphonate, GC purity 99.5%, yield 92.0%. The product has been compared with the standard product, the GC peak time is the same, and the GC-MS (gas chromatography-mass spectrometry detection) product ion current diagram is shown figure 1 ; And the product has been confirmed by GC-MS to confirm the molecular weight is correct, see the GC-MS mass spectrum figure 2 .

Embodiment 2

[0046] Add 276 grams of diethyl phosphite, 114 grams of diethoxymethane, and 2 grams of p-toluenesulfonic acid to a dry 1000 ml glass flask. The temperature is raised to 75-80°C and reacted for 5 hours. GC detects the diethyl phosphite. After the ester reaction is complete, cool to 20°C, add 5 g of 28wt% sodium ethoxide ethanol solution to neutralize, distill at 180°C in a vacuum oil bath, collect the 130-136°C / 12 mbar fraction to obtain methylene diphosphonic acid tetraethyl 259 grams of ester, GC purity 99.3%, yield 89.9%.

Embodiment 3

[0048] Add 276 grams of diethyl phosphite, 85 grams of dimethoxymethane, and 2 grams of p-toluene sulfonic acid to a dry 1000 ml reactor, gradually increase the temperature to 45-50°C and react for 2 hours, and the atmospheric pressure to 0.5 MPa, react at 85-90°C for 3 hours, GC detects that the phosphite diester reaction is complete, cool to 20°C, add 5 g of 28wt% sodium ethoxide ethanol solution for neutralization, distill at 180°C in a vacuum oil bath, collect 130-136°C / 12 mbar fraction, 261 grams of tetraethyl methylene diphosphonate was obtained, the purity was 99.1% by GC, and the yield was 90.6%.

[0049] Example 4-Example 12: The method steps are the same as in Example 1, except that different starting materials are used to prepare tetraethyl methylene diphosphonate or tetramethyl methylene diphosphonate under different conditions , The specific raw material ratio and reaction conditions, solvent, catalyst, neutralizer, product name, GC purity, product quality and yield...

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Abstract

The invention relates to a method for cleaner production of a vitamin A intermediate product, which is used for preparing a key intermediate product methylene tetraethyl diphosphonate or methylene tetramethyl diphosphonate of vitamin A, wherein the methylene tetraethyl diphosphonate or methylene tetramethyl diphosphonate is further generated by diethoxy (dimethoxy) methane and diethyl (dimethyl) phosphite with presence of an acid catalyst. The method for the cleaner production of the vitamin A intermediate product is simple in operation, short in process, free from use of solvent, free from discharge of wastewater, economic and environment-friendly; and the product is good in selectivity, high in yield, low in cost, and convenient for industrial production.

Description

Technical field [0001] The invention relates to a clean production method of vitamin A intermediates, in particular to a method for preparing key intermediates of vitamin A, tetraethyl methylene diphosphonate and tetramethyl methylene diphosphonate, and belongs to medicine The field of biochemical technology. Background technique [0002] As early as more than 1,000 years ago, Sun Simiao of the Tang Dynasty recorded that animal liver can treat night blindness in the "Prescriptions for Qian Jin Yao". The "Neijing" also records the method of extracting vitamin A from relevant Chinese medicines to treat eye diseases (including diabetic eye diseases, etc.). In 1913, four scientists including Tavis, USA, discovered that cod liver oil could cure dry eye disease and purified a yellow viscous liquid from cod liver oil. In 1920, British scientist Manot officially named it Vitamin A, the full name is "all-trans 3,7-dimethyl-9-(2,6,6-trimethyl-1-cyclohexene)- 2,4,6,8-nonatetraen-1-ol", t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
Inventor 戚聿新陈军李新发
Owner XINFA PHARMA
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