Method for synthesizing methoxy amine hydrochlorate

Abstract

The invention discloses a synthesizing method of methoxy amine hydrochloride. Butanone oxime, water, sodium hydroxide, phase transfer catalyst are added in a reaction container; the temperature is decreased to 0-15 DEG C; a methylating reagent begins to be added; then, reaction is carried out at a temperature of 5-120 DEG C for 3-6 h; standing and layering are carried out so that an organic layerO-methyl-2-diacetylmonoxime ether and a water layer are separated; then, the O-methyl-2-diacetylmonoxime ether in the water layer is distilled and recovered under the normal pressure; the separated O-methyl-2-diacetylmonoxime ether is mixed with the distilled and recovered O-methyl-2-diacetylmonoxime ether and then with hydrochloric acid solution with a mass percentage of 30-35 percent; the mixed solution undergoes feeding and rectification at the middle of a rectifying column; butanone and methanol are recovered by the column top; methoxy amine hydrochloride solution is recovered by the column bottom; and the methoxy amine hydrochloride solution also undergo evaporation and dehydration by heating so as to obtain a hydrochloride concentrated solution thereof. The synthesizing method is simple, generates a small amount of three wastes and improves the operation environment and the yield rate.

Description

technical field [0001] The invention relates to the technical field of compound synthesis methods, in particular to a method for synthesizing methoxyamine hydrochloride. Background technique [0002] Methoxylamine hydrochloride, also known as o-methylarginine hydrochloride, is an important chemical product and pharmaceutical intermediate, which can be used in color photography and film printing, as a reducing agent in the organic synthesis industry to prepare oximes, and in medicine. Used in the production of sulfamethoxazole, ethinoxazole, hydroxyurea, cefuroxime, etc. [0003] The methods currently used for the synthesis of methoxyamine hydrochloride include: Ji Yongxin (Chemistry and Adhesion, 2001, 5, 200-202) introduced such a synthetic route: use sodium bisulfite and sulfur dioxide to react with sodium nitrite Hydroxylamine sodium sulfite, then methylated, hydrolyzed, neutralized to form a salt. This process uses liquid sulfur dioxide and sodium nitrite, which is hig...

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Problems solved by technology

This process uses liquid sulfur dioxide and sodium nitrite, which is highly toxic and polluting. At the same time, more than ten tons of waste water containing a large amount of sodium sulfate will be produced to produce a ton of products, and a large amount of nitrogen oxides and other waste gases will be produced. Therefore, it is safe and environmentally friendly. There are certain problems

[0004] Han Shidong et al. (Zhejiang Chemical Industry, 2005, 36(9), 14~16) and Pan Zhongwen et al. (Fine Chemical Intermediates, 2007, 37(6), 17~18, 21) introduced a method using acetone oxime ether and O- The process of synthesizing alkoxyamines by hydrolysis of alkylphthalimides, the hydrolysis of acetone oxime ether requires continuous distillation of acetone in the rectification tower to promote the reaction, and azeotropic dehydrating agents such as toluene, hexane, etc. Organic solvents help dehydration, and it is not easy to control the side reactions in the hydrolysis process, resulting in a decrease in yield and an increase in cost

[0005] Li Wenxiao et al. (Fine Chemical Raw Materials and Intermediates, 2007, 22-23, 29) introduced the use of ethyl acetate and hydroxylamine for oximation to protect N, followed by ethylation with diethyl sulfate to form ether and then The process of preparing ethoxylamine by hydrolysis, in which impurities such as N-ethyl-O-ethylamine must be removed by distillation under reduced pressure after ethylation, and the product ethoxylamine is obtained by adding acid hydrolysis, neutralization, and distillation. The yield is 85%, and the mole fraction of the product is 98%, but there are problems that it is difficult to achieve the effect of distillation and removal of impurities, and the process conditions such as ethylation are difficult to control

[0006] The invention patent application document with the publication number CN101357895A "Method for Synthesizing Methoxyamine Hydrochloride" is basically the same as the method introduced by Li Wenxiao et al., and there are also problems of large investment and high recovery cost for ethanol and acetic acid recovery

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