Synthesis method of drug intermediate 3-methoxy-2-thiophenecarboxaldehyde

Abstract

The invention discloses a synthesis method of a drug intermediate 3-methoxy-2-thiophenecarboxaldehyde, wherein the synthesis method includes the following steps: adding 3-methoxy-2-methanol-thiopheneand a decane solution into a reaction container, increasing the temperature of the solution, controlling the stirring speed, adding aluminum isopropanol and an aqueous solution, and continuing to react; adding a phosphotungstic acid powder and a potassium chloride solution in batch, controlling the temperature, continuing to react, reducing the temperature, allowing to stand, stratifying the solution, washing with a sodium sulfate solution, washing with a sulfolane solution, recrystallizing in a hexanol solution, dehydrating with a dehydrating agent, and thus obtaining the finished product 3-methoxy-2-thiophenecarboxaldehyde.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a synthesis method of a pharmaceutical intermediate 3-methoxy-2-thiophenecarbaldehyde. Background technique [0002] 3-methoxy-2-thiophenecarbaldehyde is mainly used as a pharmaceutical intermediate, and most of the existing synthetic methods use 3-methoxy-2-thiophenecarbohydrazide, ammonia water, potassium ferricyanide and other raw materials as reactants. The ammonia water used in the synthesis method is irritating to the nose, throat and lungs after inhalation, causing cough, shortness of breath and asthma; it can cause suffocation and death due to laryngeal edema; pulmonary edema can occur and cause death. Ammonia splashed into the eyes can cause serious damage, even blindness, and skin contact can cause burns. Chronic effects: Repeated exposure to low concentrations can cause bronchitis. Repeated skin cont...

AI Technical Summary

Problems solved by technology

[0002] 3-methoxy-2-thiophenecarbaldehyde is mainly used as a pharmaceutical intermediate, and most of the existing synthetic methods use 3-methoxy-2-thiophenecarbohydrazide, ammonia water, potassium ferricyanide and other raw materials as reactants. The ammonia water used in the synthesis method is irritating to the nose, throat and lungs after inhalation, causing cough, shortness of breath and asthma; it can cause suffocation and death due to laryngeal edema; pulmonary edema can occur and cause death

Ammonia and potassium ferricyanide in the synthetic raw materials will increase the risk factor of the synthetic process, endanger the health of operators, and be unfavorable for safe production. The above factors cause many shortcomings in this synthetic method, so it is necessary to propose a new synthetic method

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