Metaraminol bitartrate synthesis method

A technology for the synthesis of metaraminol bitartrate and a synthesis method, which is applied in the field of synthesis of metaraminol bitartrate, can solve problems such as poor synthesis quality and complex synthesis methods, and achieve the effects of less synthesis steps, high preparation efficiency, and easy reaction operation

Inactive Publication Date: 2019-02-01
HUBEI TIANSHU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the synthetic method of metaraminol bi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The present invention proposes a kind of synthetic method of metaraminol bitartrate, comprises the steps:

[0018] S1: Preparation of raw materials: Dissolve sodium bisulfite in water, add m-nitrobenzaldehyde, stir and dissolve at 40°C to obtain an adduct, add ferrous sulfate to the adduct, and heat at 90°C for 3 hours , and continue stirring during the heating process to reduce it to amino, cool the reducing solution to below 15°C, add sodium nitrite solution dropwise for diazotization, and then hydrolyze at 100°C to obtain m-hydroxybenzaldehyde, and the resulting m-hydroxybenzaldehyde is hydrolyzed Hydroxybenzaldehyde is decolorized by activated carbon, and the m-hydroxybenzaldehyde solution after decolorization is heated and crystallized at 120°C;

[0019] S2: Addition reaction: place the crystallized m-hydroxybenzaldehyde in the synthesis bottle, add nitroethane and sodium thiosulfate titration solution into the synthesis bottle at the same time, and pour into the s...

Embodiment 2

[0028] The present invention proposes a kind of synthetic method of metaraminol bitartrate, comprises the steps:

[0029] S1: Preparation of raw materials: Dissolve sodium bisulfite in water, add m-nitrobenzaldehyde, stir and dissolve at 55°C to obtain an adduct, add ferrous sulfate to the adduct, and heat at 100°C for 2 hours at the same time , and continue stirring during the heating process to reduce it to an amino compound, cool the reducing solution to below 15°C, add sodium nitrite solution dropwise for diazotization, and then hydrolyze at 105°C to obtain m-hydroxybenzaldehyde, and the resulting m-hydroxybenzaldehyde is hydrolyzed Hydroxybenzaldehyde is decolorized by activated carbon, and the m-hydroxybenzaldehyde solution after decolorization is heated and crystallized at 160°C;

[0030] S2: Addition reaction: place the crystallized m-hydroxybenzaldehyde in the synthesis bottle, add nitroethane and sodium thiosulfate titration solution into the synthesis bottle at the ...

Embodiment 3

[0039] The present invention proposes a kind of synthetic method of metaraminol bitartrate, comprises the steps:

[0040] S1: Preparation of raw materials: Dissolve sodium bisulfite in water, add m-nitrobenzaldehyde, stir and dissolve at 70°C to obtain an adduct, add ferrous sulfate to the adduct, and heat at 120°C for 1 hour at the same time , and continue stirring during the heating process to reduce it to an amino compound, cool the reducing solution to below 15°C, add sodium nitrite solution dropwise for diazotization, and then hydrolyze at 110°C to obtain m-hydroxybenzaldehyde. Hydroxybenzaldehyde is decolorized by activated carbon, and the m-hydroxybenzaldehyde solution after decolorization is heated and crystallized at 200°C;

[0041] S2: Addition reaction: place the crystallized m-hydroxybenzaldehyde in a synthesis bottle, add nitroethane and sodium thiosulfate titration solution to the synthesis bottle at the same time, and pour 100°C into the synthesis bottle to heat...

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Abstract

The invention discloses a metaraminol bitartrate synthesis method, which comprises: S1, raw material preparation: dissolving sodium hydrogen sulfite in water, adding m-nitrobenzaldehyde, stirring anddissolving at a temperature of 40-70 DEG C to obtain an adduct, adding ferrous sulfate to the adduct, heating for 1-3 h at a temperature of 90-120 DEG C while continuously stirring to reduce to obtainan amino product, cooling the reducing solution to a temperature of below 15 DEG C, adding a sodium nitrite solution in a dropwise manner, carrying out diazotization, hydrolyzing at a temperature of100-110 DEG C to obtain m-hydroxybenzaldehyde, decolorizing the m-hydroxybenzaldehyde with active carbon, and carrying out heating crystallization on the decolorized m-hydroxybenzaldehyde solution ata temperature of 120-200 DEG C; S2, addition reaction; S3, preliminary crystallization; S4, salt formation; S5, synthesis reaction; and S6, recrystallization. According to the present invention, the synthesis method has characteristics of easily-available raw materials, simple preparation, less synthesis steps, high preparation efficiency, high enantioselectivity, high yield, and easily-controlled, safe and reliable reaction operation.

Description

technical field [0001] The invention relates to the technical field of metaraminol bitartrate, in particular to a synthesis method of metaraminol bitartrate. Background technique [0002] Metaraminol Bitartrate is the bitartrate of Metaraminol Bitartrate. It is an α-adrenergic receptor agonist developed by FreseniusKabi Company in the United States. It mainly acts on α-receptors. It is suitable for the treatment of early shock and prevention of spinal canal internal resistance. Acute hypotension during delayed anesthesia. In the prior art, the synthesis method of metaraminol bitartrate is complicated and the synthesis quality is poor. Contents of the invention [0003] The present invention proposes a kind of synthetic method of metaraminol bitartrate, to solve the problem that proposes in the above-mentioned background technology. [0004] The present invention proposes a kind of synthetic method of metaraminol bitartrate, comprises the steps: [0005] S1: Preparation ...

Claims

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Application Information

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IPC IPC(8): C07C215/60C07C213/02C07C213/10C07C59/255C07C51/41C07C51/43C07C223/06C07C221/00C07C245/20C07C47/565C07C45/64C07C205/17C07C201/12
CPCC07C45/64C07C51/412C07C51/43C07C201/12C07C213/02C07C213/10C07C221/00C07C245/20C07C223/06C07C47/565C07C205/17C07C215/60C07C59/255
Inventor 刘云龙
Owner HUBEI TIANSHU PHARMA CO LTD
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