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Preparation process for environment-friendly semisynthetic caffeine

A technology of caffeine and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of low reaction efficiency and low reaction efficiency, and achieve the effects of improving utilization rate, low cost and obvious reduction of production cost

Active Publication Date: 2016-02-03
CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because theophylline or theophylline sodium have very low solubility in organic solvents, the reaction efficiency is low, and the solid-liquid two-phase reaction system is the only choice under the condition of no choice, so the solid-liquid two-phase reaction efficiency Far less effective than liquid-liquid two-phase reaction

Method used

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  • Preparation process for environment-friendly semisynthetic caffeine
  • Preparation process for environment-friendly semisynthetic caffeine
  • Preparation process for environment-friendly semisynthetic caffeine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: Add 1 mole of sodium theophylline, 2 moles of DMC, 800 grams of water, 10 grams of NaY and 10 grams of Turkish red oil in a 2-liter three-neck flask with a mechanical stirrer, a reflux condenser and a thermometer device. The reaction was heated to reflux under stirring conditions. After 5 hours of reaction, carry out TLC detection (petroleum ether: ethyl acetate 5:1). When the transformation of theophylline sodium is complete, stop the reaction, and naturally cool down. When the room temperature is reached, the solid in the reaction is separated by suction filtration. The crude product can be obtained by organic solvent acetic acid Extract the product with ethyl ester or methanol to separate the catalyst NaY. After distilling off the solvent, 161 grams of earthy red caffeine crude product is obtained, with a yield of 83%. The product is dried and has a melting point of 233-238°C. The crude product is oxidized and decolorized by potassium permanganate to ob...

Embodiment 2

[0050] Embodiment 2: In 2 liters of there-necked flasks with mechanical stirrer, reflux condenser and thermometer device, add respectively 1 mole of theophylline sodium, 2 moles of DMC, the mother liquor in Example 1, 10 grams of NaY. The reaction was heated to reflux under stirring conditions. After 5 hours of reaction, carry out TLC detection (petroleum ether: ethyl acetate 5:1). When the transformation of theophylline sodium is complete, stop the reaction, and naturally cool down. When the room temperature is reached, the solid in the reaction is separated by suction filtration. The crude product can be obtained by organic solvent acetic acid Extract the product with ethyl ester or methanol to separate the catalyst NaY. After distilling off the solvent, 180 grams of earthy red caffeine crude product is obtained, with a yield of 92.7%. The melting point of the product is 230-240° C. after drying.

Embodiment 3

[0051] Embodiment 3: Add 1 mole of theophylline, 2 moles of DMC, 800 milliliters of water, 10 grams of DABCO-10 grams of NaY respectively in a 2-liter three-necked flask with a mechanical stirrer, a reflux condenser and a thermometer device (i.e. 1:1 compound) complex and 10 grams of Turkish red oil. Heating to reflux reaction was carried out under the condition of continuing stirring. After 5 hours of reaction, carry out TLC detection (petroleum ether: ethyl acetate 5:1). When the transformation of theophylline sodium is complete, stop the reaction, and naturally cool down. When the room temperature is reached, the solid in the reaction is separated by suction filtration. The crude product can be obtained by organic solvent acetic acid Extract the product with ethyl ester or methanol to separate the catalyst NaY. After distilling off the solvent, 186 grams of earthy red caffeine crude product is obtained, with a yield of 95.8%. The melting point of the product is 233-239° C. ...

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Abstract

The invention relates to a preparation process for environment-friendly semisynthetic caffeine. According to the preparation process, preparation is carried out under the specific conditions like a temperature range of 90 to 160 DEG C, usage of an alkaline substance Y type zeolite as a catalyst, addition of a proper amount of surfactant substance Turkey red oil as an emulsifier and the like, and dimethyl carbonate (DMC) is used to replace limited toxic dimethyl sulphate (DMS); reaction yield is as high as 97.8%; and the quality of a caffeine product meets requirements.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis process of caffeine. Background technique [0002] Caffeine (eaffeine), the chemical name is 3,7-dihydro-1,3,7-trimethyl-IH-trimethyl-2,6-diketone (3,7-dihydro-1,3,7- trimethyl-IH-purine-2,6-dione), also known as l,3,7-trimethylxanthine (1,3,7-Trimethylxanthine), caffeine (Guaranine), tea element (Theine), its Latin The name is eaerrinum. There are two forms of caffeine: water-free and water-containing products. The water-containing products contain a molecule of crystal water. Their molecular structural formulas, molecular weights and CAS numbers are: [0003] The molecular structure of crystal-free water is as follows: [0004] [0005] Molecular weight: 194.19; CASNO.: 58-08-2. [0006] The molecular structure of crystalline water is as follows: [0007] [0008] Molecular weight: 212.21; CASNO.: 5743-12-4. [0009] Caffeine is white or very slightly ye...

Claims

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Application Information

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IPC IPC(8): C07D473/12
CPCC07D473/12
Inventor 杨丰科李红芳李俊峰
Owner CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD
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