CN107188822A

CN107188822A - A kind of preparation method of nardil

Info

Publication number: CN107188822A
Application number: CN201710370171.7A
Authority: CN
Inventors: 王伟
Original assignee: Chongqing Jinshan Science and Technology Co Ltd
Current assignee: Chongqing Jinshan Science and Technology Co Ltd
Priority date: 2017-05-23
Filing date: 2017-05-23
Publication date: 2017-09-22

Abstract

The invention provides a kind of preparation method of nardil, this method is using 2 phenyl ethylamines, ketazine and water as raw material, and reaction at a certain temperature prepares nardil.Excessive ketazine and water are added during the course of the reaction so that the 2 phenyl ethylamines reaction in reaction system is complete, reaction removes water and ketazine after terminating using vacuum distillation, solid matter through recrystallization, dry after obtain nardil.The inventive method technique is simple, and course of reaction does not produce salt-containing organic wastewater, and product post processing is simple, and reaction yield is high, and waste discharge is few, and the ammonia and acetone that by-product is reclaimed can be back to synthesis ketazine, and production cost is low, is a kind of environmental type production technology.

Description

A kind of preparation method of nardil

Technical field

The invention belongs to chemosynthesis technical field, and in particular to a kind of preparation method of nardil.

Background technology

Nardil also known as 2- phenethyl hydrazines, are white needle-like crystals, are soluble in alcohol, ether, are dissolved in water.Nardil is a kind of anti- Depressed manic medicine, belongs to MAOI, and antidepressant effect is similar to Nialamide, can reduce intracerebral catecholamine（Go Methylepinephrine, dopamine, serotonin）Degraded, increase changes of Catecholamine Content, thus rise antidepressant effect.

At present, the preparation method of nardil mainly has two kinds：Method one：Benzyl carbinol generates nardil salt with hydrochloric acid hydrazine reaction Hydrochlorate, is then neutralized with sodium hydroxide（Alkali is analysed）It is made nardil, then is extracted with ether, obtains nardil finished product after rectifying；Side Method two：2- chloroethyls benzene and excess hydrazine hydrate reaction generation nardil and hydrazine hydrochloride, then extracted with ether, obtain benzene second after rectifying Hydrazine finished product.The shortcoming that prior art prepares nardil presence is as follows：（1）Method one is neutralized with sodium hydroxide（Alkali is analysed）Produce benzene A large amount of salt-containing organic wastewaters can be produced during ethyl hydrazine, the intractability of the waste water is big, processing cost is high, waste discharge amount Greatly, environmental pollution is easily caused；（2）The hydrazine hydrochloride of by-product need to be neutralized to obtain hydrazine hydrate with sodium hydroxide in method two, then will Hydrazine hydrate is used to prepare nardil, and this can equally produce a large amount of salt-containing organic wastewaters difficult to deal with；（3）Method one and method two All it is that, using expensive hydrazine hydrate or hydrazine hydrochloride as raw material, product post processing is complicated, and total recovery is low（With hydrazine hydrate or hydrazine hydrochloride Rate of collecting is less than 80%）, production cost is higher.

The content of the invention

In order to overcome the disadvantages mentioned above that prior art is present, the invention provides a kind of technique is simple, reaction yield is high, raw The production nardil novel preparation method that cost is low, environmental pollution is small.

The technical solution adopted by the present invention is：Using 2- phenyl ethylamines, ketazine and water as raw material, react at a certain temperature Prepare nardil.Excessive ketazine and water are added during the course of the reaction so that the 2- phenyl ethylamines in reaction system have reacted Entirely, the acetone and ammonia produced in course of reaction can be used for synthesis ketazine after being reclaimed using rectifier unit and ammonia recovery unit, Reaction removes water and ketazine after terminating using vacuum distillation, and solid matter obtains nardil after recrystallizing, drying.

The specific processing step of the inventive method is as follows：2- phenyl ethylamines, ketazine and water are put into reactor, opened Stirring, is heated to 100 DEG C~120 DEG C and is reacted, and the gas for reacting generation is introduced into rectifying column, in tower top temperature 54 DEG C~58 DEG C at extraction acetone and ammonia is put into ammonia recovery unit, azeotropic enters the ketazine of rectifying column together with water vapour Flowed back to after condensed in reactor and continue to participate in reaction, terminate reaction after rectifying tower top is released without ammonia, by reactor Water and remaining ketazine are all steamed with negative pressure, the solid matter in reactor with Diethyl ether recrystallization, dry after obtain benzene Ethyl hydrazine finished product.

In above-mentioned steps, the mol ratio of 2- phenyl ethylamines and ketazine is 1: 1.5~2,2- phenyl ethylamines and the mass ratio of water For 1: 1~1.5.Its reaction equation is as follows：

Compared with prior art, beneficial effects of the present invention and advantage are as follows：

The present invention prepares nardil by raw material of ketazine that is with low cost, being readily synthesized, and technique is simple, and course of reaction is not produced Raw salt-containing organic wastewater, product post processing is simple, and reaction yield is high（With ketazine rate of collecting more than 90%）, discarded object row Put few, the ammonia and acetone that by-product is reclaimed can be back to synthesis ketazine, and production cost is low, be a kind of environmental type production work Skill.

Embodiment

Embodiment 1

2- phenyl ethylamines 121.2g, ketazine 168g and water 122ml are put into four mouthfuls of burnings with stirring, thermometer and rectifier unit In bottle, the receiver top of rectifying column connects a conduit to absorb ammonia；Open stirring, by solution be heated to 100 DEG C~ 120 DEG C, after the gas that reaction is produced enters rectifying column, extraction acetone and ammonia is reclaimed at 54 DEG C~58 DEG C of column top temperature, Flowed back to after water vapour and ketazine in rectifying column are condensed in flask and continue to participate in reaction, when rectifying column receiver is without ammonia Terminate reaction after releasing, the water in flask and remaining ketazine are all steamed with negative pressure, the solid matter in flask is used Nardil 127.9g is obtained after Diethyl ether recrystallization, drying.

Embodiment 2

2- phenyl ethylamines 121.2g, ketazine 196g and water 150ml are put into four mouthfuls of burnings with stirring, thermometer and rectifier unit In bottle, the receiver top of rectifying column connects a conduit to absorb ammonia；Open stirring, by solution be heated to 100 DEG C~ 120 DEG C, after the gas that reaction is produced enters rectifying column, extraction acetone and ammonia is reclaimed at 54 DEG C~58 DEG C of column top temperature, Flowed back to after water vapour and ketazine in rectifying column are condensed in flask and continue to participate in reaction, when rectifying column receiver is without ammonia Terminate reaction after releasing, the water in flask and remaining ketazine are all steamed with negative pressure, the solid matter in flask is used Nardil 128.6g is obtained after Diethyl ether recrystallization, drying.

Embodiment 3

2- phenyl ethylamines 121.2g, ketazine 224g and water 180ml are put into four mouthfuls of burnings with stirring, thermometer and rectifier unit In bottle, the receiver top of rectifying column connects a conduit to absorb ammonia；Open stirring, by solution be heated to 100 DEG C~ 120 DEG C, after the gas that reaction is produced enters rectifying column, extraction acetone and ammonia is reclaimed at 54 DEG C~58 DEG C of column top temperature, Flowed back to after water vapour and ketazine in rectifying column are condensed in flask and continue to participate in reaction, when rectifying column receiver is without ammonia Terminate reaction after releasing, the water in flask and remaining ketazine are all steamed with negative pressure, the solid matter in flask is used Nardil 129.3g is obtained after Diethyl ether recrystallization, drying.

Claims

1. a kind of preparation method of nardil, it is characterised in that comprise the following steps：2- phenyl ethylamines, ketazine and water are put into In reactor, stirring is opened, 100 DEG C~120 DEG C is heated to and is reacted, the gas for reacting generation is introduced into rectifying column In, extraction acetone and ammonia is put into ammonia recovery unit at 54 DEG C~58 DEG C of tower top temperature, azeotropic enters together with water vapour Flowed back to after the ketazine of rectifying column is condensed in reactor and continue to participate in reaction, terminate anti-after rectifying tower top is released without ammonia Should, the water in reactor and remaining ketazine are all steamed with negative pressure, the solid matter in reactor is tied again with ether Nardil finished product is obtained after brilliant, dry；In above-mentioned steps, the mol ratio of 2- phenyl ethylamines and ketazine is 1: 1.5~2,2- benzene The mass ratio of ethamine and water is 1: 1~1.5.