Synthesis process of quinoline medical intermediate

Abstract

The invention discloses a synthesis process of a quinoline medical intermediate. The method comprises the following steps: step 1, when the room temperature is 20 DEG C, dissolving SM in ethanol, adding ethyl acetoacetate, anhydrous magnesium sulfate and L acetic acid, and ending the reaction after 18 hours; step 2, cooling the solution to room temperature, performing filtering, draining a filter cake, performing leaching with ethanol, and concentrating the filtrate to be dry to obtain a reddish brown liquid; step 3, when the temperature of the reddish brown liquid in the step 2 is raised to 70 DEG C, pouring 75% sulfuric acid into a 50L reaction kettle, and when raising the temperature to 80 DEG C, slowly dropping SM into a reaction bottle; step 4, performing stirring for 30 minutes after the addition is finished, dropwise adding 10 L of water when no raw materials are detected, and performing treatment after the addition is finished; and step 5, cooling the solution to the room temperature, then adding 10 L of water, and adjusting the pH value of the solution to 7-8. According to the synthesis process of the quinoline medical intermediate, operation simplification is achieved, ring closing operation can be directly conducted under the condition of crude products in the first-step reaction, the yield is not affected, the solvent is simple and cheap, and operation is convenient.

Description

technical field [0001] The invention relates to a synthesis method of quinoline, in particular to a synthesis process of quinoline series pharmaceutical intermediates, and belongs to the technical field of quinoline synthesis. Background technique [0002] Quinoline, also known as benzopyridine and azine, is a heterocyclic aromatic organic compound and a colorless hygroscopic liquid with a strong odor. Its molecular formula is C9H7N. Exposing quinoline to light will slowly turn pale yellow and further brown. Quinoline is slightly soluble in water, but readily soluble in many organic solvents. Quinoline is an important intermediate in metallurgy, dyestuff, polymer and agrochemical industries. It can also be used as a disinfectant, preservative and solvent. [0003] There are not many manufacturers of quinoline series products in the market. One of the main problems is that the process of closing the ring requires a very high temperature. In the actual scale-up process, many...

AI Technical Summary

Problems solved by technology

[0003] There are not many manufacturers of quinoline series products in the market. One of the main problems is that the process of closing the ring requires a very high temperature. In the actual scale-up process, many factories consider safety factors and generally do not choose to carry out the temperature above 200 degrees. Synthetic operation, and the conventional solvents are high boiling point solvents such as diphenyl ether and biphenyl eutectic. In use, the temperature needs to be heated to 250 degrees Celsius to achieve ring closure. Usually, due to excessive temperature, some products will decompose or have isomerization The production of bodies requires special equipment in the mass production process to facilitate operation

The product of the ring closure step is charred and difficult to purify

Images