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ChemicalBook CAS DataBase List Retinoic acid

Retinoic acid synthesis

9synthesis methods
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Yield:302-79-4 90.2% Reaction Conditions: with tris(triphenylphosphine)ruthenium(II) chloride;oxygen;bis-(3-methyl-1-imidazolyl)ethylene tetrafluoroborate in hexane at 50; under 760.051 Torr; for 3 h;Darkness;Reagent/catalyst; Steps:

1.2

2) Take 1L of bis- (3-methyl-1-imidazole) ethylene tetrafluoroborate and add RuCl2 (PPh3) 3 (the added amount is 1mol% of tretinoin), stir to dissolve,Then add 2mol of retinoid acid in the dark,The reaction was carried out in an oxygen atmosphere of 1 atm at 50 ° C for 3 hours. After the reaction, n-hexane was added for extraction,The extract was collected and dried to obtain crude tretinoin.The crude retinoic acid product obtained above was suspended in absolute ethanol, heated to 80 ° C under reflux to dissolve, and then slowly cooled to 10 ° C with stirring, allowed to stand, filtered, washed with a small amount of ethanol, and dried in vacuo to obtain pure retinoic acid product. The total yield is 90.2% and the purity is 99%.The structure identification of the prepared tretinoin was carried out, and the obtained compound was indeed the target compound. 

References: CN111087335,2020,A Location in patent:Paragraph 0020; 0029; 0031-0032; 0043; 0047; 0051

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