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Method for the continuous synthesis of monoalkyl-hydrazines with a functionalised alkyl group

A synthetic method and technology of alkylhydrazine, applied in organic chemistry, preparation of hydrazine, etc., can solve problems such as expensive operation, inability to prepare alkylhydrazine, and inability to prepare monosubstituted alkylhydrazine, so as to avoid complicated treatment and excellent Selective, low-cost effects

Inactive Publication Date: 2007-01-10
CENT NAT DE LA RECHERCHE SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method cannot be used to prepare all alkylhydrazines, especially monosubstituted alkylhydrazines
Also, the processing of the synthetic solution requires the extraction of water and subsequent amine, which requires expensive operations

Method used

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  • Method for the continuous synthesis of monoalkyl-hydrazines with a functionalised alkyl group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0048] Example: Continuous preparation of monoallylhydrazine

[0049] [31] All indicated quantities conform to the unit system and are relative to 1 liter of hypochlorous acid injected.

[0050] [32] One liter of sodium hypochlorite prepared by diluting a 50% high-concentration hypochlorous acid solution (100-120° chlorine titer, [NaOCl]=2.14mol / l, [NaCl]=0.85mol / l after dilution) Solution and one liter of the solution containing the ammonia of 3.60mol / l concentration and the solution of the ammonium chloride of 2.38mol / l concentration respectively with the rate of 5ml / min (that is the hypochlorous acid solution of the 48 ° chlorine titer of 6g / min and 5.05g NH / min 3 +NH 4 Cl ammonia mixture) was continuously injected into the stirred reactor (R1).

[0051] [33] The temperature in the reactor is maintained at -8--11°C, and the reaction pH is about 10. When removed from R1, a solution of monochloramine with a concentration greater than 1 mol / l is obtained, which corresponds...

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Abstract

The invention relates to a method for the continuous synthesis of monoalkyl-hydrazines with a functionalised alkyl group. The inventive method is characterised in that it comprises a step consisting in demixing a solution containing the synthesised monoalkyl-hydrazine, by reacting an anhydrous amine with monochloramine, in an organic phase and an aqueous phase with the addition of anhydrous sodium hydroxide. The invention can be used to obtain perfect selectivity in relation to monoalkyl-hydrazine without the presence of the di- and tri-substituted forms thereof. According to the invention, the starting amine which has not reacted is collected and reused directly without any additional treatment.

Description

technical field [0001] [1] The present invention relates to a continuous synthesis method of monoalkylhydrazines having functionalized alkyl groups. Background technique [0002] [2] In the context of the present invention, "monoalkylhydrazine" is understood as having the chemical formula NH 2 Any hydrazine of -NH-R, wherein R represents a functionalized alkyl group, that is, contains at least one functional group selected from the following groups: unsaturated carbon-carbon (such as allylhydrazine) or carbon-nitrogen groups, hydroxyl (such as 2-hydroxyethylhydrazine), alkoxy (such as 2-methoxyethylhydrazine) or phenoxy (such as Ph-O-CH 2 -CH 2 -NH-NH 2 ), carboxylic acid groups, tertiary amine functional groups (such as (Me) 2 N-CH 2 -CH 2 -NH-NH 2 ) or phenyl (such as Ph-CH 2 -NH-NH 2 ). [0003] [3] Monoalkylhydrazine, especially allylhydrazine, is a compound often used as a pharmaceutical intermediate. [0004] [4] Currently, the only synthetic methods describ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/16C07C241/02
CPCC07C241/02C07C243/16C07C243/10
Inventor 亨利·德拉吕塞西尔·科拉斯-杜里舍雅克·贝尔泰菲利普·勒朗
Owner CENT NAT DE LA RECHERCHE SCI