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The preparation method of 5-bromo-n-pentanoyl bromide

A technology of bromo-n-valeryl bromide and bromo-n-valeric acid, which is applied in the field of preparation of organic compounds, and can solve the problems of large dosage and no compound synthesis process given

Active Publication Date: 2019-12-13
DALIAN JOIN KING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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

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  • The preparation method of 5-bromo-n-pentanoyl bromide
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  • The preparation method of 5-bromo-n-pentanoyl bromide

Examples

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Embodiment 1

[0023] The preparation method of 5-bromo-n-pentanoyl bromide is specifically divided into three steps, and the reaction formula is as follows:

[0024]

[0025] 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

[0034] Prepare 5-bromo-n-pentanoyl bromide according to the method described in Example 1, and the process conditions of concrete changes are as follows:

[0035] Synthesis of the first step intermediate I: prepared according to Example 1, or outsourced;

[0036] The synthesis of the second step intermediate II: experiment according to the conditions in the following table:

[0037]

[0038]The synthesis of the third step final product 5-bromo-n-pentanoyl bromide: experiment according to the conditions in the following table,

[0039] Intermediate I% Intermediate II% Reaction temperature / ℃ Response time / hour Intermediate I% Target product % Example 2 13 84 room temperature 0.5 -- 94 Example 3 12 82 room temperature 0.5 2 90 Example 4 11 85 room temperature 1.5 -- 97 Example 5 9 69 room temperature 0.5 5 80 Example 6 12 64 room temperature 0.5 1 76 Example 7 35 56 room temperature 0.5...

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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

[0001] 1. Technical field: [0002] The present invention relates to a method for the preparation of organic compounds. [0003] 2. Background technology: [0004] 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. [0005] 3. Contents of the invention: [0006] 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. [0007] 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: [0008] The synthesis of the first ste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/50C07C51/58
Inventor 王海瑛王永灿
Owner DALIAN JOIN KING FINE CHEM CO LTD
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