Synthesis
Cool the mixture of methylene chloride and phosphorous trichloride to -5 , in which the volume ratio of methylene chloride to phosphorous trichloride was 10:3, under stirring, the mixture of B, triethylamine and methylene chloride was added dropwise at the same time with the dosage of 0.1 g/mL of B, 0.5 g/mL of triethylamine, and 2 times the volume of methylene chloride, respectively; the temperature was controlled to be between -5 and 5 , and the temperature was controlled at -5 , and the temperature was controlled at 5. Minutes, add 5 times the volume of aqueous hydrochloric acid pH 3 solution to wash, partition, aqueous layer with dichloromethane extraction, discard the organic layer, aqueous layer with isobutanol extraction, combined isobutanol layer, dry and concentrated, add petroleum ether, precipitate a solid after filtration to obtain solid C;
Product D dissolved in 3 times the weight of water, stirring dropwise addition of saturated sodium carbonate solution, to pH 7, continue to add 3 times the volume of acetone, to no longer precipitate solids, filtration, filter cake dissolved in methanol, filtration and drying with anhydrous sodium sulfate, evaporation of methanol, the solid was recrystallized with acetone - water (acetone and water volume ratio of 3:7) to obtain the product of sodium sulfate of methanaphthalene hydroquinone.
The yield of sodium menaquinone sulfate was 90.0%, and the purity was 99.1%.
Sodium menadione sulfate was added to magnesium stearate and pressed into tablets according to the common method used in pharmacy, and the content of sodium menadione sulfate was 5mg/tablet.
