Preparation method of isopropyl acetoacetate

A technology of isopropyl acetoacetate and isopropanol, which is applied in the field of preparation of pesticides and pharmaceutical synthetic raw materials, can solve the problems of low product yield, high cost, low yield, etc., to improve reaction yield and reduce the amount of waste , Improve the effect of product quality

Inactive Publication Date: 2018-05-04
SHANDONG HUIHAI PHARMA & CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 2: Diketene method: Diketene and isopropanol are used as starting materials to synthesize isopropyl acetoacetate through esterification under the action of sulfuric acid. The raw materials are cheap and easy to obtain and become the mainstream production method, but it also has its own inherent The disadvantage is that the prod

Method used

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  • Preparation method of isopropyl acetoacetate
  • Preparation method of isopropyl acetoacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 160g of isopropanol and 0.104g of catalyst into the reaction kettle, start stirring, add 208g of diketene dropwise into the reaction kettle, keep the temperature of the reaction process at 60±20°C, keep warm for 0.5h after the addition of diketene is completed, and obtain acetoacetate iso The crude propyl ester is obtained after rectification, with a yield of 93.5% and a product purity of 98.5%.

Embodiment 2

[0023] Add 160g of isopropanol and 0.024g of catalyst into the reaction kettle, start stirring, drop 240g of diketene into the reaction kettle, keep the temperature of the reaction process at 60±20°C, keep warm for 0.5h after the addition of diketene is completed, and obtain acetoacetate iso The crude propyl ester is obtained after rectification, with a yield of 93.2% and a product purity of 98.4%.

Embodiment 3

[0025] Add 160g of isopropanol and 1.12g of catalyst into the reaction kettle, start stirring, add 224g of diketene dropwise into the reaction kettle, keep the temperature of the reaction process at 60±20°C, keep warm for 0.5h after the addition of diketene is completed, and obtain isoacetoacetate The crude propyl ester is obtained after rectification, with a yield of 93.7% and a product purity of 98.6%.

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Abstract

The invention relates to a preparation method of isopropyl acetoacetate. The preparation method comprises the following steps of using diketene and islpropanol as starting materials, performing esterification to synthesize coarse isopropyl acetoacetate under catalysis action of a self-made catalyst with graphene as a carrier, then rectifying to obtain the finished product. Due to use of the self-made catalyst with graphene as the carrier, the reaction is thorough and is easy to control; generated byproduct isopropyl ether in the coarse isopropyl acetoacetate is controlled less than 1%, so thatthe reaction yield and product quality are improved, the yield and product purity of isopropyl acetoacetate are 93% or more and 98% or more respectively, up by 10% and 15% respectively in comparisonwith the method using sulfuric acid as the catalyst; the use ratio of the raw materials is improved, waste materials are reduced, environment protection investment is reduced, and the product cost islowered.

Description

technical field [0001] The present invention relates to a kind of preparation method of pesticide and medicine synthesis raw material, more specifically relate to a kind of preparation method of isopropyl acetoacetate. Background technique [0002] Isopropyl acetoacetate is a colorless, transparent, oily liquid with an aromatic odor. It is mainly used in the fields of synthetic medicine and synthetic pesticides, and has broad market prospects. [0003] After searching relevant information and comparative analysis, there are mainly two processing routes for synthesizing isopropyl acetoacetate both at home and abroad at present, as follows: [0004] 1: tert-butyl acetate method: using benzene as a solvent, two molecules of tert-butyl acetate are condensed in the presence of metal sodium to obtain isopropyl acetoacetate and isopropanol in one step, although the conversion rate of this route is relatively high (70%- 85%), but use highly toxic compound solvent benzene and strong...

Claims

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Application Information

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IPC IPC(8): C07C67/46C07C67/54C07C69/72
CPCC07C67/46C07C67/54C07C69/72
Inventor 于西波张忠政李华振张国辉侯绪会张翠翠
Owner SHANDONG HUIHAI PHARMA & CHEM
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