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Chemical synthesis of 1-chloroformyl-4-methylpiperazine hydrochloride

A methylpiperazine hydrochloride, a technology for chemical synthesis, applied in the direction of organic chemistry, etc., can solve the problems of storage and transportation difficulties, poor thermal stability, and difficulty in refining, and achieves good product quality, short reaction period, and reaction yield. high effect

Inactive Publication Date: 2005-11-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since phosgene (COCl 2 ) is a highly toxic gas that is strictly controlled and restricted internationally, and there are great safety hazards in the process of production, transportation, storage and use
Diphosgene is a liquid, and its safety is greater than that of phosgene, but its thermal stability is poor and its refining is difficult. There are still major security risks in the process

Method used

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  • Chemical synthesis of 1-chloroformyl-4-methylpiperazine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The molar ratio of feeding is N-methylpiperazine:bis(trichloromethyl)carbonate is 1:0.30, the organic solvent is benzene, and its consumption is 5 times of the mass of N-methylpiperazine.

[0011] In a 1000mL four-necked flask equipped with a thermometer, a reflux condenser, a constant pressure dropping funnel and mechanical stirring, 90g of bis(trichloromethyl)carbonate and 250g of benzene were added. Start stirring, and add dropwise a benzene solution containing 100 g (1 mol) of N-methylpiperazine. After the addition was completed, the temperature was raised to 80°C, and the reaction was kept under steady reflux for 5 hours. After the reaction was completed, benzene was recovered by distillation under reduced pressure, and the residue was recrystallized with acetone to obtain 130 g of white solid 1-chloroformyl-4-methylpiperazine hydrochloride. The melting point is 229-230° C., the yield is 75%, and the content of the product determined by liquid chromatography is 98....

Embodiment 2

[0013] The molar ratio of feeding is N-methylpiperazine:bis(trichloromethyl)carbonate is 1:0.5, the organic solvent is benzene, and its consumption is 5 times of the mass of N-methylpiperazine.

[0014] Other same example 1. The yield is 82%, and the product content is 99.3%.

Embodiment 3

[0016] The molar ratio of feeding is N-methylpiperazine:bis(trichloromethyl)carbonate is 1:0.75, the organic solvent is benzene, and its consumption is 5 times of the mass of N-methylpiperazine.

[0017] Other same example 1. The yield is 85%, and the product content is 99.0%.

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PUM

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Abstract

1-chloroformyl-4-methylpiperazine hydrochloride is an important organic synthesis intermediate, and the present invention uses bis(trichloromethyl)carbonate and N-methylpiperazine as raw materials to react in an organic solvent have to. The chemical synthesis method eliminates safety hazards and sources of three wastes from the source of the process, and is a 1-chloroformyl-4-methylpiperazine with easy-to-obtain raw materials, safe and reliable production, high reaction yield, low production cost, and basically no three wastes Synthesis method of hydrochloride.

Description

technical field [0001] The invention relates to a chemical synthesis of 1-chloroformyl-4-methylpiperazine hydrochloride prepared by directly replacing phosgene with bis(trichloromethyl)carbonate or reacting diphosgene with N-methylpiperazine method. 1-Chloroformyl-4-methylpiperazine hydrochloride is mainly used in the synthesis of medicines, pesticides and dyes, such as USP 5981500, USP 4407797, USP4327095, USP3966931, etc. Background technique [0002] Before the present invention was made, the existing main method of chemically synthesizing 1-chloroformyl-4-methylpiperazine hydrochloride was synthesized by N-methylpiperazine and phosgene or diphosgene as raw materials, such as JP 8971865 et al. Since phosgene (COCl 2 ) is a highly toxic gas that is strictly controlled and restricted internationally, and there are great potential safety hazards in the production, transportation, storage and use. Diphosgene is a liquid, and its safety is greater than that of phosgene, bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/16
Inventor 苏为科叶徐君梁现蕊张建萍谢媛媛李永曙
Owner ZHEJIANG UNIV OF TECH
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