127697-58-9Relevant articles and documents
Synthetic method of retinoic acid derivative Am580
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, (2021/03/13)
The invention discloses a synthetic method of retinoic acid derivative Am580, which comprises: stirring a solution of 2, 5-dimethyl hexane-2, 5-diol in concentrated HCl for 30 min, introducing HCl gasinto the system, carrying out a reaction for 3 h, performing stirring until the system becomes a two-phase mixture, performing cooling to a room temperature, performing filtering to obtain a light pink solid, washing the solid with water, performing recrystallizing in methanol, and performing filtering to obtain an intermediate 3 which is a white solid; dissolving 2, 5-dichloro-2, 5-dimethylhexane in an organic solvent, adding AlCl3 into the solution according to a molar ratio of the 2, 5-dichloro-2, 5-dimethylhexane to the AlCl3 of 1: 0.1-1: 0.2, performing heating to 100-120 DEG C, performing stirring for 16 hours, quenching the reaction by using 3M HCl, performing extracting by using normal hexane, and performing distilling under reduced pressure to remove the solvent to obtain a colorless oily matter intermediate 4. The method has the beneficial effects that the yield of each step is relatively high, the post-treatment is simple, and the industrial production is easier; reaction conditions and a solvent system are optimized for the Friedel-Crafts reaction and the oxidation reaction, and industrial production is better facilitated.