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A technique for the synthesis of isocytosine, which is applied in the field of chemical synthesis, can solve problems such as environmental hazards, failure to achieve, and unsatisfactory yields, and achieve the effects of wide sources, reduced by-product formation, and increased yields
Inactive Publication Date: 2017-11-24
NINGXIA MEDICAL UNIV
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Problems solved by technology
[0005] This synthetic method also has weak points: one is that the toluene used in the synthetic method has strong toxicity, which has certain harm to people's health, especially the skin, mucous membranes and central nervous system of the human body, and also has serious harm to the environment. The air, water environment and water sources may cause serious pollution. In addition, according to the "Regulations on the Safety Management of Hazardous Chemicals" and "Regulations on the Administration of Precursor Chemicals", toluene belongs to the third category of precursor chemicals, so in terms of the source of toluene There are many restrictions; the second is that the yield of the synthetic method is not ideal enough, and the details of the synthetic method such as heating temperature are not detailed enough to be disclosed in the article. After many tests, the highest yield obtained is 67%, which does not reach the article. Compared with the yield of more than 80% in foreign research, there is still a certain gap
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Embodiment 1
[0026] The synthesis of embodiment one isocytosine
[0027] Step a), the synthesis of ethyl hydroxyacrylate sodium salt, the synthetic formula is:
[0028]
[0029] Put 10.5g (0.194mol) of catalyst sodium methoxide and 10.5ml (0.13mol) of ethyl formate as reactant into the reaction kettle in sequence at -5~0°C. ml (0.14mol) was slowly added dropwise into the reactor, refluxed for 4 hours, and cooled to room temperature to obtain the intermediate sodium salt of ethyl hydroxyacrylate.
[0030] Step b), the synthesis of isocytosine, the synthetic formula is:
[0031]
[0032] Add an appropriate amount of methanol to the sodium salt of the intermediate ethyl hydroxyacrylate prepared in the previous step to dissolve it just enough, add catalyst 3A molecular sieve, add 8.7g (0.09mol) of guanidine hydrochloride, heat to 90°C and reflux for 3h, cool to room temperature, and evaporate the mixture to dryness Add an appropriate amount of pure water until the mixture is just disso...
Embodiment 2
[0036] The synthesis of embodiment two isocytosine
[0037] Step a), the synthesis of ethyl hydroxyacrylate sodium salt, the synthetic formula is:
[0038]
[0039] Put 3.45g (0.15mol) of catalyst sodium and 8.67ml (0.12mol) of ethyl formate reactant into the reaction kettle at -5~0°C in sequence, after stirring evenly, heat to 75°C and keep it under reflux, and add 14.6ml of ethyl acetate (0.15mol) was slowly added dropwise into the reactor, refluxed for 4h, and cooled to room temperature to obtain the intermediate sodium salt of ethyl hydroxyacrylate.
[0040] Step b), the synthesis of isocytosine, the synthetic formula is:
[0041]
[0042] Add an appropriate amount of n-butanol to the sodium salt of the intermediate hydroxyethyl acrylate prepared in the previous step to dissolve it just enough, add catalyst 3A molecular sieve, put in 11.46 g (0.12 mol) of guanidine hydrochloride, heat to 90 ° C and reflux for 3 h, cool to room temperature, evaporate The residual so...
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Abstract
The invention provides a synthesis method of isocytosine. The synthesis method comprises the following steps: step a), synthesizing sodium hydroxyethyl acrylate: after mixing ethyl formate and a catalyst according a certain mole ratio under the condition that the temperature is -5 DEG C to 0 DEG C, heating and reflowing; slowly dropwise adding ethyl acetate to obtain the sodium hydroxyethyl acrylate; step b), synthesizing the isocytosine: adding guanidine hydrochloride for synthesizing the isocytosine into the prepared sodium hydroxyethyl acrylate; after heating and reflowing, evaporating to dry a residual solvent; adding water into a concentrated object obtained by evaporation and dissolving; then regulating the pH (Potential of Hydrogen) to be neutral with acid; then evaporating the obtained solution to be dry and removing unreacted raw materials to obtain an isocytosine pure product, and drying. According to the method provided by the invention, the raw materials do not contain chemicals which easily cause toxin, have a wide source and do not cause damages to human bodies and environments; furthermore, reactants are mixed under the condition that the temperature is -5 DEG C to 0 DEG C in a synthesis process of the sodium hydroxyethyl acrylate, the generation of byproducts can be reduced and the yield of the isocytosine is improved.
Description
technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing isocytosine. Background technique [0002] Isocytosine, chemical name: 2-amino-4-hydroxypyrimidine, is a key intermediate for the design and synthesis of pyrimidine compounds. In recent years, high-efficiency and low-toxic drugs containing pyrimidine structural units emerge in an endless stream, especially the skeleton of isocytosine exists in the molecular structure of many anti-tumor drugs, such as acyclovir (Acyclovir), Gleevec (Gleevec) and so on. With the development of the pharmaceutical industry, the demand for pyrimidine drugs will increase, and the export is promising, but there is still a lack of industrial production in China. With the deepening of application research, isocytosine will become a hot product that attracts much attention. At present, there is no extensive research on the new path of isocytosine synthesis in China. T...
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