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Synthesis process of 5-chloro-2-pentanone

A synthesis process and pentanone technology are applied in the field of synthesis technology of 5-chloro-2-pentanone, can solve the problems of high price of raw materials, harsh reaction conditions and high price of raw materials, achieve large interlayer distance and easy availability of raw materials , the effect of cheap raw materials

Pending Publication Date: 2022-06-07
ANHUI JIXI COUNTY HUIHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 4 synthetic routes of 5-chloro-2-pentanone have been reported in the prior art: 1) take 5-chloropentyne as a raw material, and then use gold as a catalyst to react under acidic conditions to obtain the target product, and the yield is relatively high. Low and the price of raw materials is high; 2) with 4-chlorobutyryl chloride as the starting raw material, the intermediate amide is reacted with triphenylphosphine bromide to obtain 5-chloro-2-pentanone. The method uses butyllithium, Raw materials such as triphenylphosphine bromide have harsh reaction conditions and are not suitable for industrialized production; 3) using acetyl n-propanol as a starting material, the target product is obtained through chlorination, but the raw material price is higher
This shows that the current 5-chloro-2-pentanone synthesis method is not suitable for large-scale industrial production due to the limitations of raw material sources, reaction conditions and low conversion rates.

Method used

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  • Synthesis process of 5-chloro-2-pentanone
  • Synthesis process of 5-chloro-2-pentanone
  • Synthesis process of 5-chloro-2-pentanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The composite catalyst comprises the following steps to prepare:

[0030] D1, will 1.57gZn (NO 3 ) 2 ·6H 2 O and 0.95gAl (NO 3 ) 3 ·9H 2 The mixture of O was dissolved in 45 g of deionized water, then 10.3 g of sodium salt solution of tetrakis (4-sulfonic acid phenyl) porphyrin cobalt was added, and the pH value was maintained at 8.5 by continuously dripping 18 g of 0.1 mol / L NaOH solution, Stir at 80°C for 24h, filter the product, wash with distilled water at 80°C, and finally dry at room temperature to obtain the catalyst precursor;

[0031] D2. After stirring and mixing 0.55 mmol of N-hydroxyphthalimide and 28 mg of the catalyst precursor uniformly, a composite catalyst is obtained.

Embodiment 2

[0033] The composite catalyst comprises the following steps to prepare:

[0034] D1. 1.67g Zn(NO 3 ) 2 ·6H 2 O and 1.05g Al (NO 3 ) 3 ·9H 2 The mixture of O was dissolved in 50 g of deionized water, and then 11.2 g of sodium salt solution of tetrakis(4-sulfonic acid phenyl) porphyrin cobalt was added, and the pH value was maintained at 8.5 by continuous dropwise addition of 21 g of 0.1 mol / L NaOH solution. Stir at 80°C for 24h, filter the product, wash with distilled water at 80°C, and finally dry at room temperature to obtain the catalyst precursor;

[0035] D2. After stirring and mixing 0.61 mmol of N-hydroxyphthalimide and 30 mg of the catalyst precursor uniformly, a composite catalyst is obtained.

Embodiment 3

[0037] The composite catalyst comprises the following steps to prepare:

[0038] D1. 1.72g Zn(NO 3 ) 2 ·6H 2 O and 1.15g Al (NO3 ) 3 ·9H 2 The mixture of O was dissolved in 55g of deionized water, then 12.5g of sodium salt solution of tetrakis (4-sulfonic acid phenyl) porphyrin cobalt was added, and the pH value was maintained at 8.5 by continuous dropwise addition of 25g of 0.1mol / L NaOH solution, Stir at 80°C for 24h, filter the product, wash with distilled water at 80°C, and finally dry at room temperature to obtain the catalyst precursor;

[0039] D2. After stirring and mixing 0.64 mmol of N-hydroxyphthalimide and 32 mg of catalyst precursor uniformly, a composite catalyst is obtained.

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Abstract

The invention relates to a synthesis process of 5-chloro-2-pentanone, and belongs to the technical field of medicine synthesis, the synthesis process comprises the following steps: S1, dissolving methyl 4-hydroxyvalerate in tetrahydrofuran, and adding 1-(2-chloroethoxy)-2-methoxyethane to obtain a composition A; s2, dissolving the composition A in tetrahydrofuran, adding zinc chloride, and adding sodium borohydride to obtain a composition B; s3, mixing the composition B with concentrated hydrochloric acid, and adding anhydrous zinc chloride to obtain a composition C; and S4, dissolving the composition C in tetrahydrofuran, adding a composite catalyst, introducing oxygen, filtering, extracting, drying and distilling to obtain the 5-chloro-2-pentanone. According to the technical scheme, 4-hydroxyl methyl valerate is used as an initial raw material for synthesizing 5-chloro-2-pentanone, and a target compound is prepared through five steps of reaction including hydroxyl protection, ester group'one-pot method 'deprotection, chlorination and hydroxyl oxidation.

Description

Technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and specifically relates to a synthesis process of 5-chloro-2-pentanone. Background technique [0002] 5-Chloro-2-pentanone is an important pharmaceutical and chemical intermediate. It can be used to prepare important pharmaceutical intermediates such as 5-diethylamino-2-pentanone and cyclopropylamine, and is used in chloroquine phosphate and quinolone drugs. of production. In recent years, the demand for this product has increased dramatically, and it is of great significance to conduct research on its synthesis process to improve its production capacity and process level. [0003] Four synthetic routes for 5-chloro-2-pentanone have been reported in the prior art: 1) Using 5-chloropentyne as the raw material, gold as the catalyst, and reacting under acidic conditions to obtain the target product, not only the yield is relatively high; Low and the price of raw materials used is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/38C07C49/16
CPCC07C45/38C07C67/31C07C41/26C07C29/10C07C49/16C07C69/14C07C43/137C07C31/36
Inventor 洪建敏朱良德程上飞方斌程典武
Owner ANHUI JIXI COUNTY HUIHUANG CHEM
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