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
View PDF2 Cites 1 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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, in particular 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 quinolones. production. In recent years, the demand for this product has increased sharply, and it is of great significance to carry out research on its synthesis process to improve its production capacity and technological level. [0003] 4 synthetic routes of 5-chloro-2-pentanone are reported in the prior art: 1) take 5-chloropentyne as raw material, then take gold as catalyzer, react under acidic conditions to obtain the target product, not only the yield is relatively high; 2) Take 4-chlorobutyryl chloride as the starting material, first obtain t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap