Method for synthesizing dihydrojasmones

Abstract

The invention discloses a method for synthesizing dihydrojasmones, wherein the method comprises the following steps: S1, adding a sulfuric acid solution into a reaction kettle provided with a mechanical stirrer, a water segregator and a reflux condenser pipe, uniformly stirring, and carrying out heating reflux; S2, dropwise adding 3-oxo-2-pentyl-1-cyclopentene-1-acetic acid into the reaction kettle with the dropwise adding rate being 14-17 g / min, then performing a reaction for 4-6 h under the reflux condition of 40-100 DEG C, standing and layering, and obtaining an organic phase 1 after a water phase 1 is separated out; and S3, adding a sodium sulfate aqueous solution into the organic phase 1, stirring for 10-30 min, performing standing for layering, separating out a water phase 2 to obtain an organic phase 2, performing reduced pressure distillation on the organic phase 2, and collecting fractions so as to obtain dihydrojasmones. Compared with a traditional process, the method has theadvantages that reaction conditions are simple, synthesis steps are simple and convenient, reaction reagents are cheap and easy to obtain and can be recycled for multiple times, cost is reduced, andwastewater treatment is greatly reduced.

Description

technical field [0001] The invention relates to the field of perfume synthesis, in particular to a method for synthesizing dihydrojasmone. Background technique [0002] Dihydrojasmone is a kind of spice. Its aroma is strong green and floral, fresh and fruity. In fruity and floral fragrances, it can enhance the momentum of floral fragrances, such as in jasmine, ylang-ylang, lily of the valley, magnolia, tuberose and other floral fragrances. A small amount is shared with fruity notes to produce a pleasant top note. It has the ability to enhance the aroma of bergamot, lavender, lavender, clares and other herbal scents. [0003] At present, dihydrojasmone has multiple synthetic methods, (1) using undecylenic acid as a raw material, in the presence of phosphoric acid, obtained through decompression cyclization; (2) 2,5-undecanedione in Condensation in sodium hydroxide ethanol solution, or condensation of acrylate and heavy octanol under the catalysis of peroxide, and then dehy...

AI Technical Summary

Problems solved by technology

[0003] At present, dihydrojasmone has multiple synthetic methods, (1) using undecylenic acid as a raw material, in the presence of phosphoric acid, obtained through decompression cyclization; (2) 2,5-undecanedione in Condensation in sodium hydroxide ethanol solution, or condensation of acrylate and heavy octanol under the catalysis of peroxide, and then dehydration and rearrangement to obtain dihydrojasmone; (3) using cyclopentenedione as raw material, in sulfuric acid In the medium, it is obtained by reacting with amyl Grignard reagent; the above method has cumbersome steps, serious waste water, low yield, and is difficult to meet industrial needs

Images