Cinnamyl Cinnamate CAS 122-69-0

Currently, there are numerous approaches for preparing Cinnamyl Cinnamate:
1. Obtained from the lasting reaction of ethanol and cinnamic aldehyde in anhydrous ether.

2. Usage warm caustic antacids remedy to treat all-natural styrax balsam and Peru balsam to remove cinnamic cinnamate. The price of cinnamon cinnamate created by this method is high, raw materials are tough to find, the procedure is complex, and it seriously pollutes the setting.

3. CN200810046866.0. The innovation title “A prep work approach of cinnamyl cinnamate” discloses the response of cinnamic acid and thionyl chloride to prepare cinnamoyl chloride, and after that reacts with cinnamyl alcohol in the existence of an organic solvent to manufacture cinnamyl cinnamate. Although this synthesis approach has a reasonably straightforward procedure, it eats a great deal of solvent, has several by-products, and has a low return. The product is challenging to cleanse, and the natural solvent N,N-dimethylaniline used in this preparation approach has a pungent odor. Stronger flavors inevitably cause a product that doesn’t have a pure scent.

4. Preparation of cinnamon ester by transesterification of ethyl cinnamate and cinnamyl alcohol. The reaction is typically executed under high pressure. After the response, it is straight decolorized with triggered carbon and recrystallized several times to acquire the final product. This process has troubles such as lengthy reaction cycle, numerous spin-offs, problem in formation, significant air pollution, and low return.

The preparation method includes the following steps:
( 1 )Reaction.

In an oil bath, mix methyl cinnamate, cinnamyl alcohol and potassium carbonate in a mass proportion of 1:1 to 2:0.05 to 0.1. The resulting mix is warmed to 120 to 160 ° C with stirring, and responds at this temperature. For 1 to 3 hours, the methanol created by the reaction will certainly distill out as the temperature rises. When the methanol no longer distills out, quit heating and lower the temperature level to 80 ° C to obtain a response remedy containing cinnamon cinnamate;.

( 2) Cleaning and recycling.

Include water and ethyl acetate to the reaction service having cinnamon ester acquired symphonious (1 ), after that stir and wash till the water stage is neutral, separate the water phase from the oil phase, eliminate the water stage, and the oil stage is in vacuum cleaner. The ethyl acetate solvent is gotten rid of by heating under the problems of -0.096 MPa and temperature 45 ° C, and after that distilled under decreased stress under the problems of pressure 0.1 ~ 0.2 KPa and temperature level 195 ~ 205 ° C to acquire unrefined cinnamon ester;.

( 3) Formation.

The crude Cinnamyl Cinnamate obtained in step (2) is recrystallized in ethanol at a temperature level of 0 to -10 ° C, the crystals are divided, and then dried to obtain cinnamyl cinnamate as a white strong.

Compared with the prior art, the synthesis method of cinnamyl cinnamate of today development utilizes methyl cinnamate and cinnamyl alcohol as response basic materials, and transesterification reaction happens under the catalysis of potassium carbonate. During the response process, the generated methanol is Direct dissipation advertises the reaction to proceed in the forward instructions, enhances the conversion price of the response, reduces the reaction time, and stays clear of side response items brought on by high-pressure response. Throughout the post-treatment procedure, the here and now development adopts a vacuum distillation process to initial heavy steam out the unrefined cinnamon ester, which not just attains the effect of separation and filtration, yet additionally accomplishes the suitable effect of decolorization. Lastly, the item obtained by recrystallizing with ethanol has the advantages of pure aroma, good color and high pureness.