Preparation method of 3,7-dimethyl-3- acetylthio-6,7-epoxy-octanal

Abstract

The invention relates o a preparation method of 3,7-dimethyl-3- acetylthio-6,7-epoxy-octanal. The preparation method comprises following steps: at room temperature, in dichloromethane solvent, 3,7-dimethyl-3- acetylthio-6-octenal and 3-chloroperbenzoic acid are stirred and reacted for 4 to 10h, after reaction, a sodium hydroxide aqueous solution is adopted to adjust the pH value of an obtained reaction solution to 7, ether is adopted for extraction, an obtained organic layer is subjected to drying and filtering, an obtained filtrate is subjected to condensation so as to obtain a 3,7-dimethyl-3- acetylthio-6,7-epoxy-octanal crud product, and silica gel column separation is adopted so as to obtain the 3,7-dimethyl-3- acetylthio-6,7-epoxy-octanal high in purity. Compared with the prior art, the preparation method possesses following advantages: the preparation process is simple; operation is convenient; yield is high; the purity of finished product 3,7-dimethyl-3- acetylthio-6,7-epoxy-octanal is high; the production cost is relatively low; and the preparation method is suitable for industrialized production.

Description

[technical field]

[0001] The invention relates to a method for preparing aromatic sulfur-containing terpenes, in particular to a method for preparing 3,7-dimethyl-3-acetylmercapto-6,7-epoxy-octanal. [Background technique]

[0002] 3,7-Dimethyl-3-acetylmercapto-6,7-epoxy-octanal is a C13-norprene derivative that widely exists in various flowers, plants and tobacco. The derivative of citral is a very useful spice and pharmaceutical intermediate, especially in the spice, food and pharmaceutical industries, and has a wide range of applications.

[0003] However, there are few reports on the synthesis of 3,7-dimethyl-3-acetylmercapto-6,7-epoxy-octanal. In 2015, American scientist Robert J.Canon et al. (Identification, Synthesis, and Characterization of Novel Sulfur-Containing Volatile Compounds from the In-Deph Analysis of Lisbon Lemon Peels[J], 2015,63:1915-1931) used citral as raw material, Under the condition of 0℃, the epoxidation reaction of the double bond is carried out ...

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