Preparation process of isobutyryl ethyl acetate

A technology for the preparation of ethyl isobutyrylacetate, which is applied in the field of medicine, can solve the problems of low productivity and low purity of ethyl isobutyrylacetate, and achieve the effects of solving low productivity, improving purity, and convenient production and operation

Inactive Publication Date: 2021-02-12
门希国
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of this, the present invention aims to propose a kind of ethyl isobutyryl acetate preparation technology, has solved the present ethyl isobutyryl acetate production rate is not high when manufacturing, and the problem that purity is not high

Method used

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  • Preparation process of isobutyryl ethyl acetate
  • Preparation process of isobutyryl ethyl acetate
  • Preparation process of isobutyryl ethyl acetate

Examples

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Embodiment

[0022] A kind of preparation technology of ethyl isobutyryl acetate, concrete steps are as follows:

[0023] (1), add 125mL ethyl acetate and 13.6g (80mmol) potassium monoethyl malonate to a three-necked flask, stir and cool to 0-5°C, then add 9.12g (96mol) anhydrous magnesium chloride and 27.8mL ( 0.2mol) triethylamine, be warming up to 35 ℃ in 0.5h and stir 6h at this temperature:

[0024] (2) Cool to 0°C, add 6mL (57mmol) isobutyryl chloride dropwise at 0-5°C for about 1 hour, then react at room temperature for 12 hours:

[0025] (3) Cool to 0°C, carefully add 70mL of 13% hydrochloric acid, keep the temperature not higher than 20°C during this process:

[0026] (4), separate the organic phase, extract the aqueous layer with toluene (40mL × 3), combine the organic phases, wash with saturated sodium bicarbonate solution until neutral, then wash with 25mL saturated brine, and evaporate the solvent under reduced pressure:

[0027] (5) The crude product was distilled under red...

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Abstract

The invention provides an isobutyryl ethyl acetate preparation process which is characterized by comprising the following specific steps: step one, adding 125 mL of ethyl acetate and 13.6 g (80 mmol)of potassium mono-ethyl malonate into a three-neck flask, stirring and cooling to 0-5 DEG C, then sequentially adding 9.12 g (96 mmol) of anhydrous magnesium chloride and 27.8 mL (0.2 mol) of triethylamine, heating to 65 DEG C within 0.5 h, and stirring for 6 hours at the temperature of 65 DEG C; step two, cooling to 0 DEG C, dropwise adding 6 mL (57 mmol) of isobutyryl chloride within one hour, and carrying out reactions at the room temperature for 12 hours; step three, cooling to 0 DEG C, carefully adding 70 mL of 13% hydrochloric acid, keeping the temperature not higher than 20 DEG C in theprocess; step four, separating out an organic phase, extracting a water layer with toluene (40 mL*3), merging the organic phase, washing with a saturated sodium bicarbonate solution until the organicphase is neutral, and washing with 25 mL of saturated edible salt water, and carrying out reduced pressure distillation to remove the solvent; and step five, carrying out reduced pressure distillation on the crude product to obtain 5.5 g of colorless liquid. The method provided by the invention solves the problems of low productivity and low purity during production and manufacturing of isobutyryl ethyl acetate at present.

Description

technical field [0001] The invention belongs to the technical field of medicines, in particular to a preparation process of ethyl isobutyryl acetate. Background technique [0002] Ethyl isobutyrylacetate is an intermediate for the synthesis of drug atorvastatin, and is also an important chemical raw material. The traditional method of synthesizing ethyl isobutyrylacetate is to generate α- Ethyl isobutyrylecetoacetate is obtained by further decarboxylation, but at present this method has the problem that the productivity is not high and the purity is not high when ethyl isobutyryleacetate is produced. Contents of the invention [0003] In view of this, the present invention aims to propose a kind of ethyl isobutyryloacetate preparation technology, has solved the problem that current ethyl isobutyryleacetate is not high in production rate, and purity is not high. [0004] In order to achieve the above object, technical solution of the present invention is achieved in that w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C67/58C07C69/716C07F3/02
CPCC07C67/343C07C67/58C07F3/02
Inventor 门希国
Owner 门希国
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