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
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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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