Batch preparation method of 3,5-heptandiol dibenzoate

Abstract

The invention discloses a batch preparation method of 3,5-heptandiol dibenzoate. The 3,5-heptandiol dibenzoate is 4-substituted 3,5-heptandiol dibenzoate or unsubstituted 3,5-heptandiol dibenzoate. The batch preparation method of the 3,5-heptandiol dibenzoate comprises the following steps that 1, in the presence of a solvent and a basic catalyst, ethyl propanoate and butanone undergo an acylation reaction to produce 3,5-heptanedione, and specially, after the acylation reaction is finished, the 3,5-heptanedione is processed into a 3,5-heptanedione product by a chelating purification method, 2, in the presence of a solvent and a basic catalyst, the 3,5-heptanedione product contacts and undergoes a 4-substitution reaction with a reagent to produce 4-substituted 3,5-heptanedione, and 3, in the presence of a solvent and a basic catalyst, the 4-substituted 3,5-heptanedione or unsubstituted 3,5-heptanedione is reduced into 3,5-heptandiol by a reducing agent under alkaline conditions, and 4, in the presence of a solvent, the reduced 3,5-heptandiol reacts with a carbonyl-containing compound under certain conditions to produce the 3,5-heptandiol dibenzoate. Through the batch preparation method, cheap raw materials as initiators can be prepared into needed heptandiol dibenzoate products at a high yield. Therefore, the batch preparation method can be utilized for mass preparation of the 3,5-heptandiol dibenzoate.

Description

technical field [0001] The present invention relates to the synthesis method of organic glycol ester, especially the preparation method of 4-substituted or unsubstituted 3,5-heptanediol dibenzoate. Background technique [0002] The substituted or unsubstituted 3,5-heptanediol dibenzoate compound can be used as a catalyst component in olefin polymerization, so its synthesis method, especially the method that can be used for batch preparation, has practical significance. [0003] Chinese patent CN1454298A discloses a preparation method for such compounds used in polyolefin catalyst components, directly adopting 3,5-heptanedione or substituted 3,5-heptanedione as a starting material through reduction and esterification and several processing steps to obtain the final product. This method uses very expensive starting materials and uses relatively expensive steps such as "column chromatography" in the preparation process. Therefore, it can be judged that the above method is a l...

AI Technical Summary

Problems solved by technology

Therefore, it can be judged that the above method is a laboratory synthesis method, which is not suitable for the preparation process of this type of compound with commercial significance.

[0004] In the synthetic method disclosed in Chinese patent CN1580034A, although some cheap raw materials such as ethyl propionate and methyl ethyl ketone are used as starting materials, many high-cost treatments are still used in the preparation steps. steps and the yield of the process is also low, it can also be judged as a laboratory synthesis method and is not suitable for commercial batch preparation process