Novel method for producing theobromine with 3_methylxanthine disodium salt methylating

A technology of methylxanthine disodium salt and theobromine, applied in the direction of organic chemistry and the like, can solve the problems of incomplete reaction of raw materials, low yield, and high by-product caffeine, etc.

Inactive Publication Date: 2008-07-16
PERRIGO TRADING (SHANGHAI) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has the following weak points: raw material reaction is not thorough, yield is low (60~70%), by-product caffeine is many

Method used

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  • Novel method for producing theobromine with 3_methylxanthine disodium salt methylating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In a 500ml four-necked reaction flask with stirring, add 63 grams of 3-methylxanthine disodium salt, 304ml of acetone, and 19.1 grams of sodium carbonate, slowly raise the temperature to a slight reflux of 55°C while stirring, and add dimethyl sulfate dropwise Add 60 grams in 3.5 hours, then continue the reaction at 55°C for 0.5 hours, distill off the acetone under normal pressure, add 50ml of water, neutralize with 32% industrial hydrochloric acid at 30°C until the pH reaches 6, filter, wash with 10ml of warm water at 40°C, Drained and dried at 70°C to obtain the crude product of theobromine with a yield of 84.3%.

Embodiment 2

[0013] In a 1000ml four-necked reaction flask with stirring, add 126 grams of 3-methylxanthine disodium salt, 610ml of acetone, and 38.5 grams of sodium carbonate, slowly raise the temperature to a slight reflux of 55°C while stirring, and add dimethyl sulfate dropwise Add 120 grams in 3.5 hours, then continue the reaction at 57°C for 0.5 hours, distill off the acetone under normal pressure, add 100ml of water, neutralize with 32% hydrochloric acid at 30°C until the pH reaches 6, filter, wash with 20ml of warm water at 40°C, and pump Dry at 70°C to obtain the crude product of theobromine with a yield of 84.9%.

Embodiment 3

[0015] In a 500ml four-necked reaction flask with stirring, add 63 grams of 3-methylxanthine disodium salt, 304ml of acetone, and 31 grams of sodium carbonate, slowly raise the temperature to a slight reflux of 55°C while stirring, and dropwise add dimethyl sulfate 60 gram, after adding in 4 hours, continue to react at 60°C for 1 hour, distill off acetone under normal pressure, add 40ml of water, neutralize with 32% hydrochloric acid at 30°C until pH reaches 5, filter, wash with 15ml of warm water at 40°C, and drain The crude product of theobromine was dried at 70°C with a yield of 86.75%.

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Abstract

The invention provides a new method for preparing theobromine by 3-methyl xanthine disodium salt methylation with more production value. The theobromine is prepared by using acetone as a solvent to react with dimethyl sulfate under the existence of sodium carbonate and then acidified. The invention uses the acetone as the solvent and decreases the hydrolysis loss of the dimethyl sulfate; the sodium carbonate provides an alkaline condition for the methylation reaction and the pH value is moderate. The dimethyl sulfate is dripped to carry out the methylation reaction with the advantages of good selectivity and a yield higher than other methylation technique by more than 10 percent. The acetone is recycled and reused; the reaction is relatively complete and has little caffeine by-product; the acquired analytic content of theobromine crude product HPLC is larger than 99 percent; therefore, the invention is extremely applicable to industrial production.

Description

technical field [0001] The invention relates to a new method for preparing theobromine from methylation. Background technique [0002] Theobromine (English name: Theobromine, 3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione) is a central stimulant of xanthines, and the general preparation method is : (1) Theobromine is prepared from xanthine methylation, xanthine is dissolved in aqueous sodium hydroxide solution, pH is controlled: 8.2 to 8.5, and dimethyl sulfate is added dropwise for methylation. (2) Dissolve 3-methylxanthine in alkaline aqueous solution such as sodium hydroxide, sodium carbonate, potassium carbonate, etc., and carry out methylation by adding dimethyl sulfate dropwise. The above methods have the following disadvantages: incomplete reaction of raw materials, low yield (60-70%), and many by-products of caffeine. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing theobromine with more production value, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/12
Inventor 李兴泰舒瑞友丰宇胜杨爱荣赵丽
Owner PERRIGO TRADING (SHANGHAI) CO LTD
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