Method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride

A technology of dimethylhydroxylamine hydrochloride and methoxyamine hydrochloride, applied in the direction of organic chemistry and the like, can solve the problems of ineffective treatment of salty wastewater, serious environmental protection problems, etc., and achieves excellent product quality, low comprehensive cost, Simple and reliable process

Active Publication Date: 2016-08-17
宁波四明化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] This method will produce a large amount of saline wastewater containing sodium acetate, sodium sulfate,

Method used

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  • Method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride
  • Method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride
  • Method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0043] In a 1000mL four-neck flask reactor equipped with a thermometer, a stirrer, a constant pressure funnel, and an exhaust gas water seal, add 69 g (1 moL) of hydroxylamine hydrochloride and 69 g of water, and add 140 g of 30% NaOH (1.05 moL) dropwise at 20 to 25 ° C, Add 53g Na 2 CO 3 (0.5moL), add CH evenly within 8h 3 Cl 150.5g (3moL), while adding 30% NaOH dropwise to adjust the pH=9.5-10, then keep stirring at 2-5°C for 2h.

[0044] Change the flask to a distillation method, add 30% NaOH dropwise to adjust the pH=12, heat up and distill for 2 to 8 hours, collect the condensate with a vapor phase temperature of 60-100°C to obtain the stripping fraction, and reduce the raffinate at 75°C (vacuum-0.075MPa). Concentrate under high pressure until a large amount of salt precipitates out, filter while hot to obtain sodium chloride as a by-product, and add the mother liquor back to the next batch of raffinate to continue concentrating.

[0045] In a packed column equipped wi...

Embodiment 2

[0050] The hydroxylamine salt is changed to hydroxylamine sulfate (1mol), and the methylating reagent is changed to (CH 3 ) 2 SO 4 (2.5mol), water 160g, what reclaimed during this moment mother liquor neutralization and distillation is sodium sulfate, other is with embodiment 1. After applying the mother liquor mechanically for 5 times, the calculated total average yield of methoxyamine hydrochloride was 39%, and that of N,O-dimethylhydroxylamine hydrochloride was 31%.

Embodiment 3

[0052] The addition amount of hydroxylamine salt and methylating agent is changed into: CH of 1moL hydroxylamine hydrochloride and 1.5moL 3 Cl, and CH 3Cl was added evenly within 25 hours, and at the same time, alkali was added to adjust the pH to 11-12, and then the reaction was carried out at 35-40°C with stirring for 4 hours. Add 31% hydrochloric acid to N,O-dimethylhydroxylamine fraction to adjust pH = 2 to form a salt, add 31% hydrochloric acid to adjust pH = 2 to form a salt, both products are concentrated and crystallized under reduced pressure at 85°C, pumped after cooling Filter, recrystallize the filter cake with methanol, and dry it in vacuum at 60°C. Others are the same as in Example 1. After applying the mother liquor 5 times, the total average yield of methoxyamine hydrochloride is 50%, and N,O-dimethylhydroxylamine salt Salt is 11%.

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Abstract

The invention relates to the technical field of compound synthesis methods, particularly a method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride. The method comprises the following steps: carrying out methylation reaction on hydroxylamine salt under alkaline conditions by using a methylating agent to obtain a reaction solution containing vasoxine and N,O-dimethylhydroxylamine, rectifying to separate a vasoxine bottom solution and an N,O-dimethylhydroxylamine crude distillate, respectively adding hydrochloric acid for salification, concentrating and crystallizing under reduced pressure, cooling, carrying out vacuum filtration, recrystallizing with water or methanol, and drying to obtain the vasoxine hydrochloride product and N,O-dimethylhydroxylamine hydrochloride product. The method has the advantages of simple and reliable technique, high product quality, high total yield and low comprehensive cost, and is more friendly to the environment and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of compound synthesis methods, in particular to a method for co-producing methoxyamine hydrochloride and N,O-dimethylhydroxylamine hydrochloride. Background technique [0002] Methoxyamine hydrochloride and N,O-dimethylhydroxylamine hydrochloride are important fine chemical intermediates used in the synthesis of Weinreb amides, medicines and pesticides. The methods currently used for the synthesis of methoxyamine hydrochloride and N,O-dimethylhydroxylamine hydrochloride are: [0003] 1. Rashik method [0004] Gao Donghua et al. (Chemical Intermediates, 2003, 24, 29-31) introduced sodium nitrite and sodium bisulfite as raw materials, and the introduction of SO 2 The gas is reacted with Raschig to generate sodium salt of persinyl disulfonic acid, which is methylated with a methylating agent, then hydrolyzed, and methylated to obtain N,O-dimethylhydroxylamine. The principle of the reaction process is as follo...

Claims

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Application Information

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IPC IPC(8): C07C239/20
CPCC07C239/20
Inventor 周淑章俞阳晨段云凤石园庆柳圣境
Owner 宁波四明化工有限公司
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