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Preparation method of methoxylamine hydrochloride

A technology of methoxyamine hydrochloride and hydrochloric acid, applied in oxime preparation, organic chemistry, etc., can solve problems such as safety, environmental protection, high toxicity, serious pollution, etc., to avoid low product yield and reduce toxic gas emissions , the effect of improving production efficiency

Active Publication Date: 2020-03-27
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses sulfur dioxide and sodium nitrite, which is highly toxic and polluting, and produces a large amount of waste gas such as nitrogen oxides. Therefore, there are certain problems in safety and environmental protection, and it is not suitable for industrial production.

Method used

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  • Preparation method of methoxylamine hydrochloride
  • Preparation method of methoxylamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add butanone oxime (C4H9NO) 43.5g (0.5mol), triethylamine (C6H15N) 70.8g (0.7mol), dimethyl sulfoxide (DMSO, C2H6OS) 87g (1.1mol) to 500ml reaction flask and heat up to 60 Slowly add 82g (0.65mol) of dimethyl sulfate (C2H6O4S) dropwise at ℃ for 50min, keep warm for 6h after the dropwise addition, transfer the reaction solution into a 500ml reaction bottle, add 78.2g (0.75mol) of 35% hydrochloric acid 100 Reaction at ℃ for 120min, cooling down to room temperature, crystallization and filtration to obtain the target product with a yield of 87%.

Embodiment 2

[0030] Add 52.3g (0.6mol) of butanone oxime (C4H9NO), 98g (0.97mol) of triethylamine (C6H15N), 111g (1.42mol) of dimethyl sulfoxide (DMSO, C2H6OS) to a 500ml reaction flask and heat up to 40°C Slowly add 77.3g (0.61mol) of dimethyl sulfate (C2H6O4S) dropwise for 90min, keep warm for 7h after the dropwise addition, transfer the reaction solution into a 500ml reaction bottle, add 93.7g (0.9mol) of 35% hydrochloric acid 120 The reaction was carried out at ℃ for 140 min, then cooled down to room temperature and crystallized and filtered to obtain the target product with a yield of 91%.

Embodiment 3

[0032] Add 61g (0.7mol) of butanone oxime (C4H9NO), 106.2g (1.05mol) of triethylamine (C6H15N), 122g (1.56mol) of dimethyl sulfoxide (DMSO, C2H6OS) to a 500ml reaction flask and heat up to 75°C Slowly add 123.6g (0.98mol) of dimethyl sulfate (C2H6O4S) dropwise for 30min, keep warm for 8h after the dropwise addition, transfer the reaction solution into a 500ml reaction bottle, add 104.3g (1mol) of 35% hydrochloric acid at 95°C After reacting for 110 minutes, the product was crystallized and filtered at room temperature to obtain the target product with a yield of 89%.

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Abstract

The invention provides a preparation method of methoxylamine hydrochloride. The method comprises the following steps of adding diacetylmonoxime (C4H9NO), dimethyl sulfoxide (DMSO, C2H6OS), triethylamine (C6H15N) and a methylation reagent into a reaction vessel, and reacting at 15-75 DEG C to generate O-methyl-2-diacetylmonoxime ether. Compared with the prior art. The method has the advantages thatthe operation is simple, wastes are few, furthermore, reaction raw materials can be completely converted, a generated intermediate by-product can be decomposed into diacetylmonoxime (C4H9NO) and triethylamine (C6H15N), equivalently, no side reaction exists, the yield of synthesized methoxylamine hydrochloride is improved, the use of toxic substances such as sulfur dioxide and sodium nitrite is avoided, the emission of toxic gases such as nitric oxide is reduced, and the sustainable development of enterprises is facilitated.

Description

technical field [0001] The invention relates to a preparation method of methoxyamine hydrochloride, belonging to the technical field of pharmaceutical intermediates. Background technique [0002] Methoxyamine hydrochloride is an important pharmaceutical and chemical intermediate, mainly used in the production of cefuroxime and fenoxystrobin. Cefuroxime belongs to the cephalosporin antibiotics and is widely used because of its broad antibacterial spectrum and stability to β-lactamase. Fenoxystrobin is an excellent variety of methoxyacrylate fungicides, with high-efficiency fungicidal activity and high selectivity. With the increasing output of cefuroxime and phenoxystrobin in recent years, the demand for methoxamine hydrochloride in the international market is gradually increasing. However, the production of methoxyamine hydrochloride in my country generally has problems such as backward technology, serious three wastes, and high product cost. Therefore, it is of great sig...

Claims

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Application Information

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IPC IPC(8): C07C249/12C07C251/38
CPCC07C249/12C07C251/38
Inventor 倪欣崔宝龙尹明香宋君王炳懿
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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