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Method for synthesizing butyrolactone and butyrolactone obtained by same

A technology of lactone and ethyl crotonate, applied in the field of butyl lactone, one-step synthesis of butyl lactone, can solve the problems of many three wastes, complicated process, long synthesis steps and the like

Active Publication Date: 2012-01-11
北京北达正元科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present inventor applies the principle of free radical addition reaction to propose a new method for synthesizing butyrolactone, utilizing alcohol and 3-butenoic acid or its ester to carry out free radical addition in the presence of a free radical initiator, one step Buty lactone can be obtained, which solves the problems of long synthesis steps, complicated process and many wastes in the current synthesis of buty lactone

Method used

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  • Method for synthesizing butyrolactone and butyrolactone obtained by same
  • Method for synthesizing butyrolactone and butyrolactone obtained by same
  • Method for synthesizing butyrolactone and butyrolactone obtained by same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Synthesis of butyl-decanolactone (δ-n-pentyl-δ-valerolactone)

[0040] In a reactor equipped with a stirrer, a condenser, a thermometer, and a dropping device, add 306 g (3 moles) of 1-hexanol, heat it to 150°C, and use 7 while stirring while maintaining this temperature. A mixture of 100 g (1 mole) of methyl 3-butenoate and 97 g (0.5 mole) of tert-butyl peroxybenzoate was added dropwise every hour. After the addition, the reaction was continued at this temperature for 3 hours, and then the temperature was reduced to At room temperature, the excess 1-hexanol was recovered and then rectified under reduced pressure to obtain 132.6 g of butyrodecanolactone. The calculated yield was 78%.

Embodiment 2～ Embodiment 20

[0042] Use the type and amount of alcohol, 3-butenoic acid or its ester, and initiator shown in Table 1, and appropriately change the reaction temperature, and other conditions are the same as in Example 1 to prepare the corresponding δ-substituted-δ-pentane ester. The yield is also shown in Table 1.

[0043] Table 1

[0044]

[0045] From Table 1 above, it can be known that according to the synthesis method of the present invention, high yield of δ-substituted-δ-valerolactone can be obtained.

Embodiment 21～ Embodiment 27

[0047] As shown in Table 2, the amounts of 1-hexanol, methyl 3-butenoate, and tert-butyl peroxybenzoate and the reaction temperature were changed, and the other conditions were the same as in Example 1 to prepare buty-decanolide. The yield is also shown in Table 2.

[0048] Table 2

[0049]

[0050] From Table 2 above, it can be known that when the amounts of 1-hexanol, methyl 3-butenoate, and tert-butyl peroxybenzoate and the reaction temperature are not within the preferred range specified in the present invention, although the target product can be obtained, The yield is not very high.

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Abstract

The invention provides a method for synthesizing butyrolactone which is shown as the molecular formula (1) and butyrolactone obtained by the method. The method is characterized by obtaining the butyrolactone by carrying out free radical addition of alcohol and 3-butenoic acid or ester thereof; in the formula (1), R1 is hydrogen, a methyl or an ethyl; and R2 is a propyl, a butyl, an amyl, a hexyl,a heptyl, an octyl, a nonyl, a phenyl, a benzyl, a cyclopentyl, a cyclopentylmethyl, a cyclohexyl or a cyclohexylmethyl. The method can realize clean production and obtain high yield.

Description

Technical field [0001] The invention relates to a method for preparing butyrolactone and the butyrolactone obtained by the method. In particular, it relates to a one-step method for synthesizing butyrolactone and the butyrolactone obtained by the method. Background technique [0002] At present, regarding the preparation method of δ-substituted-δ-valerolactone, the butyrolactone, there are mainly two industrialized synthetic routes as follows. [0003] One of the synthetic routes can be represented by the following formula (I). [0004] Formula (I) [0005] It uses cyclopentanone as raw material, condenses with aldehyde under alkaline conditions to obtain 2-alkenyl cyclopentanone, then undergoes hydrogenation reduction, and finally obtains butyrolactone by oxidative ring expansion. The disadvantage of this type of method is that the synthesis step is long, the total yield is about 60%, and the operation is more complicated, and the three wastes are more generated. [0006] Another s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/30
Inventor 王川卫小广吴文德
Owner 北京北达正元科技有限公司