69413-86-1Relevant academic research and scientific papers
Synthetic method for 3-acetoxy-2-cyclohexenyl-1-one and derivatives thereof
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Paragraph 0019; 0021; 0025, (2019/10/01)
The invention discloses a synthetic method for 3-acetoxy-2-cyclohexenyl-1-one and derivatives thereof. The synthetic method comprises the following steps: (1) reacting a substance as described in thespecification with nitromethane at 110 DEG C to obtain a product I as described in the specification, wherein R in the product I is H or CH3; (2) reacting the product I of the step (1) with sodium nitrite and acetic acid at 37 DEG C to obtain a product II as described in the specification; (3) reacting the product II of the step (2) with methanol and concentrated sulfuric acid at 88 DEG C to obtain a product III as described in the specification; and (4) weighing the product III of the step (3), potassium carbonate, palladium on activated carbon and t-butyl hydroperoxide, adding the weighed materials into dichloromethane, carrying out a reaction at 0 DEG C, and allowing temperature to naturally rise to room temperature so as to obtain a product IV, wherein R in the product IV is H or CH3.The synthetic method of the invention is simpler and more efficient, and has high total yield; the toxicity of reagents used in the preparation is smaller than the toxicity of m-methoxybenzoic acid, thionyl chloride and the like used in the prior art; and the method is low in cost, simple and convenient in separation and purification, applicable to large-scale preparation and capable of realizingindustrial mass production. The synthetic method is applicable as a general synthetic method for 3-acetoxy-2-cyclohexenyl-1-one and 4-substituted derivatives thereof.
