Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparing method of 5-bromine pivaloyl bromide normal

A bromide-n-valeryl bromide, a preparation method technology, applied in the field of preparation of organic compounds, can solve the problem of not giving the compound synthesis process, large dosage, etc.

Active Publication Date: 2010-03-10
DALIAN JOIN KING FINE CHEM CO LTD
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 5-Bromo-n-pentanoyl bromide is an intermediate in pharmaceutical synthesis and is used in a huge amount. However, the product has not been reported in the literature after searching the literature. It is a new compound, and the literature does not give the specific synthesis process of the compound.

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
  • Preparing method of 5-bromine pivaloyl bromide normal
  • Preparing method of 5-bromine pivaloyl bromide normal
  • Preparing method of 5-bromine pivaloyl bromide normal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of 5-bromo-n-pentanoyl bromide is specifically divided into three steps, and the reaction formula is as follows:

[0019]

[0020] Synthesis of the first step intermediate I: Add 8.6g (85%, 0.0425mol) of m-chloroperoxybenzoic acid and 19mL of dry chloroform in a 100mL four-necked flask equipped with magnetic stirring, a thermometer and a condenser tube, and add dropwise at room temperature A solution of 2.1 g (0.025 mol) of cyclopentanone in dry chloroform (13 mL). After the dropwise addition, heat to reflux and monitor until the content of cyclopentanone is less than 0.5% to stop the reaction, then perform post-treatment, cool the reaction mixture with an ice-water bath, filter to remove the m-chlorobenzoic acid precipitate, and wash the filtrate with about 10% sodium sulfite aqueous solution until KI- Until the starch test paper does not change color, the solvent is removed by rotary evaporation, and the residue is washed with 10% potassium c...

Embodiment 2-9

[0029] Prepare 5-bromo-n-pentanoyl bromide according to the method described in Example 1, and the process conditions of concrete changes are as follows:

[0030] Synthesis of the first step intermediate I: prepared according to Example 1, or outsourced;

[0031] The synthesis of the second step intermediate II: experiment according to the conditions in the following table:

[0032]

[0033] The synthesis of the third step final product 5-bromo-n-pentanoyl bromide: experiment according to the conditions in the following table,

[0034]

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 preparing method of 5-bromine pivaloyl bromide normal, belonging to the field of synthesizing methods of compounds. The preparing method of the 5-bromine pivaloyl bromide normal comprises the following steps: (1) synthesis of a midbody I: adding raw materials, i.e. m-chloroperoxybenzoic acid and drying chloroform, into a reaction kettle, and slowly adding a drying chloroform solution containing raw material cyclopentanone at room temperature so as to obtain a crude product of the midbody I; (2) synthesis of a midbody II: adding the raw material midbody I, hydrobromicacid and sodium bromide into the reaction kettle, reacting to obtain the midbody II and directly carrying out the reaction of a next step without purification; (3) synthesis of the 5-bromine pivaloylbromide normal: adding triphenylphosphine and dichloromethane into the reaction kettle, reducing the temperature to about 0 DEG C, starting to slowly add a dichloromethane solution containing bromine, adding the raw material midbody II to react, and purifying to obtain a target product, i.e. the 5-bromine pivaloyl bromide normal. The prepared product prepared by the method has higher purity and ideal yield coefficient and is suitable for being applied to industrialized production.

Description

1. Technical field: [0001] The present invention relates to a method for the preparation of organic compounds. 2. Background technology: [0002] 5-Bromo-n-pentanoyl bromide is an intermediate in pharmaceutical synthesis and is used in a huge amount. However, this product has not been reported in the literature after searching the literature. It is a new compound, and the literature does not give the specific synthesis process of the compound. 3. Contents of the invention: [0003] The purpose of the present invention is to overcome above-mentioned insufficient problem, provide a kind of preparation method of 5-bromo-n-valeryl bromide, flow process is brief, technique is simple, product yield is high, and purity is high. [0004] The technical scheme that the present invention adopts for realizing the above object is: the preparation method of 5-bromo-n-pentanoyl bromide, specifically divides into three steps: [0005] The synthesis of the first step intermediate I: add r...

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
IPC IPC(8): C07C53/50C07C51/58
Inventor 王海瑛王永灿
Owner DALIAN JOIN KING FINE CHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com