Preparation method of metyrapone
A technology of metyrapone and acetylpyridine, applied in the field of preparation of metyrapone (1-acetone), can solve the problems of high cost, many reaction steps, cumbersome operation, etc., and achieve low cost, easy operation and short process flow Effect
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Embodiment 1
[0017] Add 1000ml of benzene and 48g of Mg powder to the reaction vessel, stir, cool to -20°C, add 20g of mercuric chloride, slowly add the mixture of 121g of 3-acetylpyridine and 100ml of benzene dropwise at -30°C, keep the reaction for 5h, then slowly Raise the temperature to reflux, react for 3 hours, and the reaction is over, cool to 50°C, add 200ml of water dropwise, stir for 30min, filter, reflux the filter cake with 200ml of benzene for 30min, filter, combine the filtrates filtered twice, discard the water layer, and recover benzene by distillation , when nearly dry, add 200ml of petroleum ether to precipitate a solid, filter to collect the solid, and dry to obtain 170g of a diol intermediate. Add the obtained diol into the reaction vessel, add 340g of concentrated sulfuric acid, slowly heat to 70°C for 3.5h, cool naturally to 40-50°C, pour the reactant into 1000ml of ice water, adjust the pH with 2N sodium hydroxide solution =8.5; extract the aqueous layer three times ...
Embodiment 2
[0019] Add 1000ml of toluene and 70g of Mg powder to the reaction vessel, stir, cool to -30°C, add 20g of mercuric chloride, slowly add the mixture of 121g of 3-acetylpyridine and 100ml of toluene dropwise at -40°C, keep the reaction for 6h, then slowly Raise the temperature to reflux, react for 3 hours, the reaction is over, cool to 50°C, add 200ml of water dropwise, stir for 30min, filter, reflux the filter cake with 200ml of toluene for 30min, filter, combine the filtrates filtered twice, discard the water layer, and recover toluene by distillation , when nearly dry, add 200ml cyclohexane to precipitate solid, filter to collect solid, and dry to obtain 165g of diol intermediate. Add the obtained diol into the reaction vessel, add 400g of 80% sulfuric acid, slowly heat to 80°C for 5 hours, cool naturally to 40-50°C, pour the reactant into 1000ml of ice water, and adjust the pH with 2N sodium hydroxide solution =8.5; the aqueous layer was extracted three times with dichlorome...
Embodiment 3
[0021] Add 1000ml of benzene and 60g of Mg powder into the reaction vessel, stir, cool to -20°C, add 30g of mercuric chloride, slowly add the mixture of 121g of 3-acetylpyridine and 100ml of benzene dropwise at -30°C, keep the reaction for 5h, then slowly Raise the temperature to reflux, react for 4 hours, and finish the reaction, cool to 50°C, add 200ml of water dropwise, stir for 30min, filter, reflux the filter cake with 200ml of benzene for 30min, filter, combine the filtrates filtered twice, discard the water layer, and recover benzene by distillation , when nearly dry, add 200ml of petroleum ether to precipitate a solid, filter to collect the solid, and dry to obtain 172g of a diol intermediate. Add the obtained diol into the reaction vessel, add 440g of 50% sulfuric acid, slowly heat to 100°C for 8 hours, cool naturally to 40-50°C, pour the reactant into 1000ml of ice water, and adjust the pH with 2N sodium hydroxide solution = 8; extract the aqueous layer three times w...
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