Method for preparing edible essence 8-mercaptomenthone from pulegone and sodium sulfide
A technology of mercaptohormone and menthone, applied in the field of food flavor preparation
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Embodiment 1
[0023] Add 300 grams of menthone, 250 grams of sodium sulfide and 1000 grams of water into the reactor, stir and mix evenly, heat to 60° C. to 70° C., and react for 15 hours under constant stirring. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35°C to 40°C to obtain 280 g of crude 8-mercaptomaleone.
[0024] Add 280 grams of 8-mercaptomaleone crude product in the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, precipitate a solid, then filter, and dry the filtered solid to constant weight to obtain the final product 8 -170 grams of mercaptomaleone, the yield is 46%, which is better than the bibliographical reports of the existing normal pressure reaction.
[0025] The NMR parameters of the prepared 8-mercaptomaleone are:
[0026] 1 H-NMR(300MHz,DMSO)δ:...
Embodiment 2
[0029] Add 300 grams of menthone, 280 grams of sodium sulfide and 1000 grams of methanol into the reactor, stir and mix evenly, heat to 60°C~70°C, add 5g of zinc chloride (Friedel-Crafts catalyst), and react under constant stirring 15 hours. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35° C. to 40° C. to obtain 320 g of crude 8-mercaptomaleone.
[0030] Add 320 grams of 8-mercaptomaleone crude product in the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, separate out the solid, then filter, and dry the filtered solid to constant weight to obtain the final product 8 -240 grams of mercaptomaleone, the yield is 65%.
Embodiment 3
[0032] Add 300 grams of menthone, 320 grams of sodium sulfide and 1200 grams of ethanol into the reactor, stir and mix evenly, heat to 60° C. to 70° C., and react for 15 hours under constant stirring. Then the above reaction mixture was diluted with water, acidified to neutral with hydrochloric acid, cooled to room temperature, filtered, and the filter cake was washed with warm water at a temperature of 35° C. to 40° C. to obtain 290 g of crude 8-mercaptomaleone.
[0033] Add 290 grams of 8-mercaptomaleone crude product in the reaction vessel, then add 400 grams of ethanol to reflux for 4 hours, then cool the solution to room temperature, precipitate a solid, then filter, and dry the filtered solid to constant weight to obtain the final product 8 - 200 grams of mercaptomaleone, the yield is 54%.
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