Batch preparation method of 3,5-heptandiol dibenzoate

A technology of heptanediol diphenylformate and heptanediol, which is applied in 3 fields, and can solve the problems of unsuitable commercial batch preparation process, high cost, and unsuitable commercial preparation process, etc.

Inactive Publication Date: 2012-04-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 e

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of 4-ethyl-3,5-heptanediol dibenzoate

[0029] (1) Add 107.5kg of NaH and 310kg of solvent THF to the reaction kettle, mix well, weigh 107.9kg of butanone and 153.7kg of ethyl propionate and mix evenly, add it to the tetrahydrofuran solution of NaH within 20h, add a small amount ethanol initiates the reaction. After the addition, the reaction system was kept at reflux (55° C.) for 2 hours, then the heating was stopped and the temperature was lowered.

[0030] Add 172.7kg of acetic acid into 500kg of ice water, stir well to form a solution, add the reaction solution to the ice solution of glacial acetic acid, keep the layers at rest, and extract the water layer with 120*2kg of ethyl acetate. The crude product of 3,5-heptanedione was obtained by distillation under reduced pressure.

[0031] (2) Prepare saturated copper acetate solution. Get the 3,5-heptanedione obtained above and add 513.25kg of 95% ethanol to dilute, then add saturated copper acetate solut...

Embodiment 2

[0037] Preparation of 3,5-heptanediol benzoate

[0038] (1) Add 0.372kg of NaOH, 21.36kg of sodium borohydride and 254L of water into the reactor, cool down to below 0°C after dissolving, start to slowly add 3,5-heptanedione pure product (the second step of embodiment 1) Step product) 84.65kg of ethanol solution (the quality of ethanol is 2.4 times of the pure product of 3,5-heptanedione), after adding, keep the temperature at 0°C for 2h, then warm up to room temperature and react for 15h. 508L of water and 125.3*3kg of chloroform were added to extract, and the organic phase was distilled to remove the solvent to obtain 3,5-heptanediol with a yield of 96.87%.

[0039] (2) Add dehydrated 3,5-heptanediol 85kg, dehydrated pyridine 122.25kg and 358kg of toluene to the reactor successively, slowly add benzoyl chloride 159.27kg, control the dropping temperature at about 50°C, and then heat up to React at about 70°C for 3 hours, filter, wash the filter cake with 45.2 kg of toluene, ...

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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...

Claims

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Application Information

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IPC IPC(8): C07C69/78C07C67/14C07C67/08C07C67/03
Inventor 郭浩然朱丽琴王红红包天舒冯静
Owner CHINA PETROLEUM & CHEM CORP
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