A kind of synthesis method of dye for blood cell analysis

A technology of blood cell analysis and synthesis method, which is applied in the field of synthesis of dyes for cell staining and blood cell analysis. It can solve the problems of low purity of target products, high raw material prices, and difficulty in removing them completely, and achieve excellent purity, rapid synthesis, and The effect of simple structure

Active Publication Date: 2019-04-12
SUZHOU COMING CHENGYE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the excellent performance and unique advantages of polymethine dyes, there are various synthetic processes for such dyes, but most of them are complicated, the raw material prices are high, the synthesis cycle is long, and the substances produced in the intermediate process are harmful to the human body. Certain damage, difficult to remove completely, the purity of the target product is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment one: the synthesis of the first intermediate product

[0024] Take 3 mmol of N,N’-dimethylformamidine into a test tube, then add 0.2 ml of acetic anhydride, stir and dissolve in an oil bath at 85°C (solution B). Then take 1mmol of 2,3-dimethylbenzothiazole methylsulfate into another test tube, add 1.5ml of acetic acid, stir and dissolve in an oil bath at 85°C (solution A).

[0025] In an oil bath at 85°C, add liquid A to liquid B drop by drop, stirring constantly. The mixed solution will gradually turn red during the dropwise addition, which means that A and B have started to react.

[0026] After the dropwise addition, the mixture was stirred and reacted in an oil bath at 85°C for 1.5 h. After the reaction, the mixture should be a dark red liquid.

[0027] After the mixture was cooled, the acetic acid and acetic anhydride in the mixture were removed by distillation under reduced pressure, and then about 20 ml of methanol was added to redissolve the mixture...

Embodiment 2

[0029] Embodiment two: the synthesis of the second intermediate product

[0030] Mix 5 mmol 1-octanol and 0.435 g pyridine with about 2 ml CH 2 Cl 2 (dichloromethane) mixed.

[0031] Mix 0.91 ml trifluoromethanesulfonic anhydride with 5 ml CH 2 Cl 2 Mix well, then store at -5°C~0°C and N 2 (Nitrogen) protection, dropwise added to 1-octanol, pyridine and CH 2 Cl 2 in the mixture. The dropwise addition process takes about 20 minutes. Too fast dropwise addition will cause the temperature to rise rapidly, which is not conducive to the progress of the reaction.

[0032] After the dropwise addition, the reaction was stirred at -10°C for 45 min. A pink product and a white solid (product of the reaction of trifluoromethanesulfonic anhydride and pyridine) appear during the reaction.

[0033] After the reaction, add an appropriate amount of CH 2 Cl 2 and water, which will dissolve the white solid, and the aqueous solution is removed after the layers are separated. The produc...

Embodiment 3

[0035] Embodiment three: the synthesis of the 3rd intermediate product

[0036] Take 3.34mmol intermediate product 2 and about 5 ml CH 2 Cl 2 (dichloromethane) mixed.

[0037] Add 3.34mmol 4-methylquinoline to the above mixture, N 2 Heated to reflux under protection for about 1 h.

[0038] Removal of CH by distillation under reduced pressure 2 Cl 2 , and then washed the product several times with anhydrous diethyl ether to remove impurities, and finally a light brown oil was obtained, which was the third intermediate product.

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PUM

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Abstract

The invention discloses a blood cell analysis dye synthesizing method. The blood cell analysis dye synthesizing method comprises the steps of synthesizing 2, 3-dimethyl-benzothiazole methyl sulfate and N, N'-dimethyl formamidine to obtain a first intermediate product; synthesizing 1-octanol and trifluoromethane sulfonic anhydride to obtain a second intermediate product; synthesizing the second intermediate product and 4-methyl-quinolin to obtain a third intermediate product; synthesizing the first intermediate product and the third intermediate product to obtain an end product. Therefore, the blood cell analysis dye synthesizing method is low in toxic and side effects, simple in raw material acquisition and structure, low in damage to synthesizing personnel and cost and short in synthetic route and can synthesize target molecules only through four steps of reaction, thereby being high in yield rate, rapid in synthesizing, excellent in purity, cost-saving, easy to industrialized and applicable to practical popularization.

Description

technical field [0001] The invention relates to a class of dyes for cell staining in the field of in vitro diagnosis, in particular to a method for synthesizing the dyes for blood cell analysis. Background technique [0002] In the early stage of cell staining, various acid-base dyes were used for staining. The accuracy of this staining method is not good, and for the classification of white blood cells in blood cells, it is necessary to show very fine internal structure differences, and then use red semiconductor lasers as light sources. capture information, so this staining method is already slightly insufficient. Now, in the field of white blood cell classification, fluorescent dye staining is widely used. [0003] In the early stage of development, the dyes used were methylene blue, brilliant phenyl blue, penonin, ethidium bromide, etc. They form complexes by intercalating or electrostatically attracting nucleic acid molecules, and the enhanced fluorescence is observed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B23/06G01N1/30
CPCC09B23/06G01N1/30G01N2001/302
Inventor 杨灵勇周丽霞李勋波苗俊杰
Owner SUZHOU COMING CHENGYE MEDICAL TECH
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