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Method for preparing N-hydroxylamine hydrochloride by hydrolyzing N-nitromethane

A technology for nitromethane and hydroxylamine hydrochloride, applied in the directions of hydroxylamine, nitrogen and non-metallic compounds, can solve the problems of complex synthesis steps, inability to large-scale production, high energy consumption, etc., and achieve easy availability of raw materials, product purity and abundance. And the effect of high yield and reasonable process

Inactive Publication Date: 2009-11-25
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Both of the above two methods have the disadvantages of complex synthesis steps, high energy consumption, and inability to produce on a large scale.

Method used

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  • Method for preparing N-hydroxylamine hydrochloride by hydrolyzing N-nitromethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A sort of 15 Preparation of N-nitromethane by hydrolysis 15 The method for N-hydroxylamine hydrochloride, the method may further comprise the steps:

[0027] (1) 15 Preparation of N-nitromethane

[0028] In a 500ml three-neck flask equipped with a magnetic stirrer, a thermometer and a dropping funnel, add an aqueous solution of anhydrous sodium carbonate (2g of anhydrous sodium carbonate dissolved in 20ml of water) and 8.8g (0.126mol) 15 N-sodium nitrite, the temperature of the mixture was lowered to 10°C, under vigorous stirring, 12ml (0.126mol) dimethyl sulfate was added dropwise within 30 minutes, after the addition was completed, the temperature was raised to 40°C, and reacted for 4h, Heating up and distilling under reduced pressure, the distilled liquid is separated by a water separator, and the lower layer is 15 N-nitromethane;

[0029] (2) 15 Preparation of N-hydroxylamine hydrochloride

[0030] In a 500ml three-neck flask equipped with magnetic stirring, ...

Embodiment 2

[0032] A sort of 15 Preparation of N-nitromethane by hydrolysis 15 The method for N-hydroxylamine hydrochloride, the method may further comprise the steps:

[0033] (1) 15 Preparation of N-nitromethane

[0034] In a 500ml three-neck flask equipped with magnetic stirring and a thermometer, add an aqueous solution of anhydrous sodium carbonate (2g of anhydrous sodium carbonate dissolved in 20ml of water) and 8.8g (0.126mol) 15 N-sodium nitrite, lower the temperature of the mixture to 5°C, under vigorous stirring, add 24g (0.252mol) chloroacetic acid within 30 minutes, after the addition, the temperature rises to 20°C, react for 6h, then heat up and distill under reduced pressure , the distilled liquid is separated by a water separator, and the lower layer is 15 N-nitromethane;

[0035] (2) 15 Preparation of N-hydroxylamine hydrochloride

[0036] In a 500ml three-neck flask equipped with magnetic stirring, thermometer and reflux condenser, add 6.83g (0.11mol) 15 N-nitrome...

Embodiment 3

[0038] A sort of 15 Preparation of N-nitromethane by hydrolysis 15 The method for N-hydroxylamine hydrochloride, the method may further comprise the steps:

[0039] (1) 15 Preparation of N-nitromethane

[0040] In a 500ml three-neck flask equipped with a magnetic stirrer, a thermometer and a dropping funnel, add an aqueous solution of anhydrous sodium carbonate (2g of anhydrous sodium carbonate dissolved in 20ml of water) and 8.8g (0.126mol) 15 N-sodium nitrite, the temperature of the mixture was lowered to 8°C, and under strong stirring, 32ml (0.252mol) methyl iodide was added dropwise within 30 minutes. Distillation under reduced pressure, the distilled liquid is separated by a water separator, and the lower layer is 15N-nitromethane;

[0041] (2) 15 Preparation of N-hydroxylamine hydrochloride

[0042] In a 500ml three-neck flask equipped with magnetic stirring, thermometer and reflux condenser, add 6.83g (0.11mol) 15 N-nitromethane, 5ml water and 24ml (0.279mol) co...

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Abstract

The invention relates to a method for preparing N-hydroxylamine hydrochloride by hydrolyzing N-nitromethane. The method adopts N-nitrite as an isotope raw material to react with a methylating agent so as to obtain the N-nitromethane, and the N-nitromethan is hydrolyzed, condensed, crystallized and filtered to obtain the N-hydroxylamine hydrochloride. Compared with the prior art, the invention has the advantages of reasonable and simple technology, easily obtained raw materials, high isotope conversion rate, product purity, abundance and yield, and the like, can prepare a great amount of N-hydroxylamine hydrochloride with high purity and high abundance and is suitable for mass production.

Description

technical field [0001] The present invention relates to 15 Preparation of N-nitromethane by hydrolysis 15 N-hydroxylamine hydrochloride method. Background technique [0002] Hydroxyamine (molecular formula NH 2 OH·HCl, colorless needle crystal, melting point 159°C) is an important organic synthesis intermediate. Used in the pharmaceutical industry for sulfamethoxazole, VB 6 , VB 12 , semi-synthetic penicillin, ibuprofen and furan drugs, etc. In chemical industry, it is used for the synthesis of new nitrile fragrances such as citronil and jasmine nitrile, and hydroxylamine perchlorate. In addition, hydroxylamine hydrochloride can also be used as auxiliary agent, reducing agent, analytical reagent, etc. [0003] 15 N-hydroxylamine hydrochloride and its derivatives such as 15 N-Suwannee River fulvic acid, 15 N-hydroxyurea, 15 N-fumarylacetone oxime and 15 N-nylon can be used as a tracer for research on the mechanism of product synthesis and the metabolism of drug pro...

Claims

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Application Information

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IPC IPC(8): C01B21/14
Inventor 刘占峰李良君杜晓宁赵诚
Owner SHANGHAI RES INST OF CHEM IND
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