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Preparation of 5,5-diethylmalonylurea

A technology of diethylmalonylurea and crude diethylmalonylurea, which is applied in the direction of organic chemistry, etc., can solve the problems that crude mothers cannot be used mechanically, poor product appearance, cumbersome operation, etc., and achieve less three wastes and lower production costs Low, high-purity effect

Active Publication Date: 2008-12-17
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has strict requirements on the reaction concentration of sodium ethoxide, and the operation is cumbersome
The reaction time is as long as 80 minutes, the energy consumption is high, the appearance of the obtained product is poor, a large amount of activated carbon is required for decolorization, the crude mother cannot be applied mechanically, there are many three wastes, and the cost is high

Method used

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  • Preparation of 5,5-diethylmalonylurea

Examples

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Effect test

Embodiment 1

[0029] Step A: adding an ethanol solution (15% by mass) containing 680 g of sodium ethylate and ethyl acetate into a reaction flask, raising the temperature to 60-65° C., and reacting for 30 minutes. Cool to below 45°C, add 800g of diethyl malonate, stir for 1 hour, add 1117g of bromoethane dropwise below 40°C. After about 7 hours of dripping, the reaction lasted for 5 hours. Gradually raise the temperature to 60-65°C for 1 hour. Ethanol and ethyl bromide were recovered by distillation to an internal temperature of 120°C. Cool down to below 40°C, and add the eliminated ethanol solution containing 84g of sodium ethoxide. Add 133g of bromoethane dropwise at below 40°C for about 4 hours, then slowly raise the temperature to 60-65°C for 1 hour. Raise the temperature and recover the solvent until the internal temperature reaches 135°C, distill the alcohol under reduced pressure when the temperature is lowered to 110°C, add water to dissolve sodium bromide when the temperature is...

Embodiment 2

[0033] Step A: Add methanol solution containing 654.2 g of sodium methoxide (25% by mass) and ethyl acetate into a reaction flask, raise the temperature to 60-65° C., and react for 30 minutes. Cool to below 45°C, add 800g dimethyl malonate, stir for 1 hour, then add 1354.3g bromoethane dropwise below 40°C. After about 7 hours of dripping, the reaction lasted for 5 hours. Gradually raise the temperature to 60-65°C for 1 hour. Recover methanol and ethyl bromide by distillation to an internal temperature of 110°C. Lower the temperature to below 40°C, add water to dissolve, statically separate the layers, evaporate the water and low boilers from the organic phase under reduced pressure to obtain a mixture of ethyl ester and heavy ester.

[0034] Add methanol solution containing 81.5g of sodium methoxide and ethyl acetate into the reaction flask, raise the temperature to 60-65°C, and react for 30 minutes. Cool to below 45°C, add the mixture of ethyl ester and heavy ester obtaine...

Embodiment 3

[0038] Step A: Add 697g of sodium ethoxide ethanol solution (20% by mass) and ethyl acetate into the reaction flask, raise the temperature to 60-65° C., and react for 30 minutes. Cool to below 45°C, add 800g of diethyl malonate, stir for 1 hour, add 1117g of bromoethane dropwise below 40°C. After about 7 hours of dripping, the reaction lasted for 5 hours. Gradually raise the temperature to 60-65°C for 1 hour. Ethanol and ethyl bromide were recovered by distillation to an internal temperature of 120°C. Lower the temperature to below 40°C, and add the eliminated ethanol solution containing 84g of sodium ethoxide. Add 133g of bromoethane dropwise at below 40°C for about 4 hours, then slowly raise the temperature to 60-65°C for 1 hour. Raise the temperature and recover the solvent until the internal temperature reaches 135°C, distill the alcohol under reduced pressure when the temperature is lowered to 110°C, add water to dissolve sodium bromide when the temperature is lowered ...

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Abstract

The invention provides a new technology for preparing 5,5-diethyl-barbituric acid compound, which comprises steps as follows: malonic ester reacts with bromoethane under the condition of 'boiling in one pot' while alcobolic solution of sodium alcoholate exists to obtain 5,5- diethyl-malonic ester; the bromoethane reacts with urea while the alcobolic solution of sodium alcoholate exists; the reaction is completed in a concentration process; after the concentration is finished, water or (mother solution) is added for dissolution and acidification is carried out to obtain crude 5,5-diethyl-barbituric acid; water or ethanol water is recrystallized to prepare 5- ethyl-5-isopentyl balbituric acid compound. The technology is stable and carbethoxy and diethyl ester are completed under the condition of 'boiling in one pot'; the synthesis reaction with the urea is completed during distillation process; the technology has no particular requirement on the concentration of sodium alcoholate and has the advantages of easily controllable reaction conditions, short reaction time, simple operation, less three wastes, good product quality, high yield, low production cost and being more applicable to industrialized production.

Description

technical field [0001] The invention relates to a new synthetic process for preparing hypnotic, sedative and anticonvulsant 5,5-diethylmalonylurea compound from malonate. Background technique [0002] 5,5-Diethylmalonylurea is mainly used for hypnosis. It is also used for administration before anesthesia and anticonvulsant. [0003] Existing preparation technology, its step is that diethyl malonate divides secondary ethylation with bromoethane in the alcoholic solution of sodium ethylate to obtain compound 5,5-diethyl malonate diethyl ester, the latter in The compound 5,5-diethylmalonylurea can be obtained by reacting with urea in the alcoholic solution of sodium ethoxide. The process has strict requirements on the reaction concentration of sodium ethoxide, and the operation is cumbersome. The reaction time is as long as 80 minutes, the energy consumption is high, the appearance of the obtained product is poor, and a large amount of activated carbon is needed for decolori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/60
Inventor 朱连博宋广慧韩勇李兴泰
Owner SHANDONG XINHUA PHARMA CO LTD
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