Method for producing dehydroepiandrosterone
A technology of dehydroepiandrosterone and production method, applied in the directions of steroids, organic chemistry, etc., can solve the problems of violent reaction, burns, fast hydrolysis reaction speed, etc., achieve stable chemical reaction, reduce production cost, and improve competitiveness Effect
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[0009] 1. Ketoxime reaction:
[0010] With ethanol 250kg (≥ 95%), pyridine 36kg (≥ 98%), pump in the tank, add hydroxylamine hydrochloride 13kg (≥ 98%), open steam and heat up 40-50 ℃, then dienolone acetate 60kg ( content ≥ 98%) was added, refluxed for 3.5 hours, cooled to 5°C, centrifuged and washed until neutral to obtain the required ketoxime.
[0011] 2. Bayesian reaction:
[0012] Put 360g of pure benzene (≥98%) and 30g of pyridine (≥98%) into the tank, raise the temperature to 40-50°C, then add the ketoxime reacted in the first step, and raise the temperature to 60°C, after the materials are completely dissolved, Cool down to 8°C, start dropping 30kg of phosphorus oxychloride (content ≥ 98%), the temperature in the tank is ≤ 16°C, finish dropping in 1.5 hours, keep warm for 3 hours, then add 90kg of hydrochloric acid solution dropwise, the content of hydrochloric acid is ≥ 30 %, the temperature in the tank is less than or equal to 25°C, after the dropwise addition is ...
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