Synthesis method of 3, 4, 7, 8-tetramethyl-1, 10-tetramethyl

Abstract

The invention provides a synthesis method of 3, 4, 7, 8-tetramethyl-1, 10-tetramethyl, which comprises the following steps of: enabling butanone and paraformaldehyde to react under the environment of potassium hydroxide carbinol solution at the temperature of 50 DEG C, dewatering by concentrated hydrochloric acid, and adding hydroquinone into solution to stop polymerizing; preparing a crude product in a distilling way under the temperature of 140 DEG C; drying, and distilling under the temperature of 97-98 DEG C; and reflowing o-phenylenediamine and 50mL of concentrated hydrochloric acid in a heating way, adding unsaturated ketone (or beta-hydroxy-ketone) under the condition of completely stirring, reacting for 16 h under the temperature of 80 DEG C, cooling, adding water to dilute, extracting by chloroform, separating out water phase, adjusting alkali by ammonia water to separate out oily matter and extracting by chloroform, concentrating the chloroform, dissolving the residue in a small number of absolute methanol, charging dried HCl gas, separating out solid hydrochloride, washing cold carbinol and diethyl ether, drying, and neutralizing by ammonia water to obtain a final product. The synthesis method is simple and convenient to operate, raw materials are low in price, and easy to obtain, the As2O5 does not need, the production cost can be greatly reduced, and the produced waste liquid is easy to process.

Description

technical field [0001] The invention relates to a synthesis method of 3,4,7,8-tetramethyl-1,10-phenanthroline. Background technique [0002] 3,4,7,8-Tetramethyl-1,10-phenanthroline is an important pharmaceutical intermediate and can be used in the synthesis of various drugs. The known literature involves a new type of anti-tumor drug Rare earth complexes, more specifically, relate to a class of rare earth complexes and their preparation methods and their application in the preparation of drugs for the treatment of tumors, using rare earth nitrates, o-phenanthroline, and 5-fluorouracil in a ratio of 1:2:3 to Absolute ethanol is used as a solvent, and reacted at 80°C under stirring to generate a new type of rare earth complex with the general formula [Ln(Phen)2(5-Fu)3(NO3)](NO3)2. Anti-tumor activity, acute toxicity, mouse sarcoma S180, mouse liver cancer HAC and anti-tumor activity in tumor-bearing nude mice have been preliminarily confirmed by a series of experiments that t...

AI Technical Summary

Problems solved by technology

[0005] Among them, the reaction product from the first step is more complicated, the whole reaction process has more side reactions and the post-treatment is more complicated, resulting in an increase in product cost, which is not conducive to industrial production.

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