Preparation method of N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt

A technology of diethylaminoacetyl and dimethylaniline, applied in the field of pharmaceutical synthesis, can solve the problems of unstable raw materials, low purity, low yield and the like, and achieves a complete reaction, high yield and purity, and economical and environmentally friendly yields. Effect

Pending Publication Date: 2021-02-23

LUNAN PHARMA GROUP CORPORATION

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Problems solved by technology

[0008] In order to solve the problems of low yield, low purity and unstable raw materials in the preparation process of QX-314-OH in the prior art, the present invention provides a new method for preparing QX-...

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Abstract

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt. The method for preparing the N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt comprises the following steps of: reacting 2-bromo-N-(2,6-dimethylphenyl)acetamide serving as a raw material with diethylaminoethanol to obtain an N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt crude product, and further stirring and crystallizing the crude product in an organic solvent to obtain the N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt pure product. The method provided by the invention has the advantages of simple reaction conditions and simplified preparation process, effectively enhances the yield and purity of the N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt, and is suitable for industrial production.

Application Domain

Organic compound preparationCarboxylic acid amides preparation

Technology Topic

ChemistryAcetamide +6

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Examples

Experimental program(7)
Comparison scheme(1)

Example Embodiment

[0026]Example 1

[0027]It is weighed 24.2 g 2-bromo-N- (2,6-dimethylphenyl) acetamide to add 100 mL of acetonitrile solution, add 21.1 g of diethyl ethanol, heating to 75 to 80 ° C. Stir, TLC detection reaction is completed. After falling to the room temperature QX-314-OH solid, the obtained QX-314-OH was added to 50 ml of heating and dissolved in 50 ml of anhydrous ether, cooled to 20 ° C holding the stirring grafting crystalline 3h, filtered, the resulting filter cake 45 ° C vacuum dry dry QX-314-OH was obtained, and the yield was 73.4%, HPLC purity 99.56%.

Example Embodiment

[0028]Example 2

[0029]It is weighed with 24.2 g of 2-bromo-N- (2,6-dimethylphenyl) acetamide to add 100 ml of toluene solution, add 21.1 g of diethylene ethanol, heating to 80 to 85 ° C, stir, TLC detection reaction After lowering to the room temperature QX-314-OH solid, the obtained QX-314-OH was added to 60 mL of methanol and heat dissolved, and the temperature was lowered to 10 ° C to heat the stirred grafting crystalline 2H, filtered, the resulting filter cake 45 ° C vacuum dry QX -314-oh, the yield was 71.7%, HPLC purity 99.48%.

Example Embodiment

[0030]Example 3

[0031]It is weighed 24.2 g 2-bromine-N- (2,6-dimethylphenyl) acetamide, adding 16 ml of acetonitrile solution, 16.4 g (0.14 mol) diethyl ethanol was added, and the reaction was stirred to 60 ~ 65 ° C, After the TLC was detected, it fell to the room temperature QX-314-OH solid, and the obtained QX-314-OH was added to 50 ml of heating and dissolved, and the temperature was lowered to 25 ° C to heat the stirred alcohol 3H, filtered, the resulting filter cake The QX-314-OH was dried in vacuo to 45 ° C, and the yield was 70.5%, HPLC purity 99.51%.

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Preparation method of N-diethylaminoacetyl-2,6-dimethylaniline quaternary ammonium salt

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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