Synthetic method for geosmin
A synthesis method and technology of geosmin, applied in the directions of hydrolysis preparation, organic chemistry, etc., can solve the problems of low overall yield, high cost, danger, etc., and achieve the effects of simple and safe operation, reduction of preparation cost, and improvement of yield
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Embodiment 1
[0028] 1) Add 2 grams of 2,6-dimethylcyclohexanone into a four-necked flask, then add 7 grams of toluene, 0.2 grams of titanium tetrachloride, and 2.8 grams of (R)-α-naphthylethylamine at room temperature , after the addition, the reaction solution was heated under reflux and stirred for 12 hours, the stirring was stopped, the toluene was evaporated to obtain the crude product, and the crude product was distilled under reduced pressure to obtain 4 . 4 g of intermediate 1, yield: 99%.
[0029] 2) Mix 4.4 g of intermediate 1 and 1.1 g of butenone at room temperature, then stir the above reaction solution at room temperature for 48 hours, stop stirring to obtain 5.4 g of intermediate 2, yield: 98%.
[0030] 3) Mix 5.4 g of intermediate 2 with 0.5 g of trifluoroacetic acid at room temperature, then stir the above reaction solution at room temperature for 1 hour, add 10 g of ethyl acetate for dilution, and wash the resulting solution with saturated sodium bicarbonate solution and w...
Embodiment 2
[0037] 1) Add 1.5 grams of 2,6-dimethylcyclohexanone into a four-necked flask, then add 5 grams of toluene, 0.15 grams of titanium tetrachloride, and 2.5 grams of (R)-α-naphthylethylamine at room temperature , after the addition was complete, the reaction solution was heated under reflux and stirred for 20 hours, the stirring was stopped, and the toluene was distilled off to obtain a crude product, which was distilled under reduced pressure to obtain 3.2 g of intermediate 1, yield: 96%.
[0038] 2) Mix 3.2 g of intermediate 1 and 0.9 g of butenone at room temperature, then stir the above reaction solution at room temperature for 60 hours, stop stirring to obtain 4 g of intermediate 2, yield: 100%.
[0039] 3) Mix 4 g of intermediate 2 with 0.3 g of trifluoroacetic acid at room temperature, then stir the above reaction solution at room temperature for 1.5 hours, add 10 g of ethyl acetate for dilution, and wash the resulting solution with saturated sodium bicarbonate solution and...
Embodiment 3
[0046] 1) Add 0.55 g of 2,6-dimethylcyclohexanone into a four-necked flask, then add 2 g of toluene, 0.08 g of titanium tetrachloride, and 1 g of (R)-α-naphthylethylamine in sequence at room temperature , after the addition was complete, the reaction solution was heated under reflux and stirred for 12 hours, the stirring was stopped, and the toluene was distilled off to obtain a crude product, which was distilled under reduced pressure to obtain 1.2 g of intermediate 1, yield: 99%.
[0047] 2) Mix 1.2 g of intermediate 1 and 0.35 g of butenone at room temperature, then stir the above reaction solution at room temperature for 72 hours, stop stirring to obtain 1.5 g of intermediate 2, yield: 100%.
[0048] 3) Mix 1.5 g of intermediate 2 with 0.1 g of trifluoroacetic acid at room temperature, then stir the above reaction solution at room temperature for 2 hours, add 5 g of ethyl acetate for dilution, and wash the resulting solution with saturated sodium bicarbonate solution and wa...
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