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Process for preparing 1.8-diazadicyclo [5,4,0] -7 undecene

A technology for diazabicyclo and acrylonitrile, which is applied in the field of preparing 1.8-diazabicyclo-7undecene, can solve the problems of high requirements on reaction equipment, low yield and the like, and achieves reduced process difficulty, high reaction yield, The effect of reducing production costs

Inactive Publication Date: 2004-11-17
吉林省石油化工设计研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that in the past, these preparation processes had problems such as low yield and high requirements for reaction equipment.

Method used

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  • Process for preparing 1.8-diazadicyclo [5,4,0] -7 undecene
  • Process for preparing 1.8-diazadicyclo [5,4,0] -7 undecene
  • Process for preparing 1.8-diazadicyclo [5,4,0] -7 undecene

Examples

Experimental program
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Effect test

Embodiment 1

[0014] In a 500ml four-neck flask, add 200g of caprolactam, 75g of toluene is heated to 55°C, 1g of sodium hydroxide catalyst is added under stirring, and 98g of acrylonitrile is added dropwise simultaneously, and the reaction temperature is controlled at 57±2°C. After toluene is cooled and filtered, the intermediate cyanoethyl caprolactam crude product is obtained, and its yield is 93%, (calculated by caprolactam), and the caprolactam conversion rate is 99%;

[0015] In a 2000ml four-neck bottle, add 600ml of distilled water, add 50g of the four-component catalyst original powder, start stirring and heat up to 90 ° C, start to drip sodium hydroxide solution, the initial concentration is 15%, a total of 200ml is added dropwise, and then 25 % sodium hydroxide solution 140ml, control the temperature at 88 ± 2 ° C, after all the sodium hydroxide solution is dripped, heat up to 94 ± 1 ° C and react for 1 hr, cool down, pour off the supernatant, wash with distilled water and anhydro...

Embodiment 2

[0019] In a 500ml four-necked flask, add 200g of caprolactam, 75g of toluene is heated to 55°C, 1g of potassium hydroxide catalyst is added under stirring, and 94g of acrylonitrile is added dropwise simultaneously, and the reaction temperature is controlled at 57±2°C. After toluene is cooled and filtered, the intermediate cyanoethyl caprolactam crude product is obtained, and its yield is 89% calculated as caprolactam, and the caprolactam conversion rate is 96%;

[0020] In a 2000ml four-necked bottle, add 600ml of distilled water, add 50g of the original four-component catalyst powder, start stirring and heat up to 85 ° C, start to drop the potassium hydroxide solution, the initial potassium hydroxide solution concentration is 15%, a total of 200ml is added dropwise, 140ml of 25% alkaline solution was added dropwise, and the temperature was controlled at 85±2°C. After all the potassium hydroxide solution was dripped, the temperature was raised to 90±1°C and reacted for 1hr. Ea...

Embodiment 3

[0024] In a 500ml four-necked flask, add 200g of caprolactam, 75g of toluene is heated to 50°C, 1g of sodium hydroxide catalyst is added under stirring, and 104g of acrylonitrile is added dropwise at the same time, and the reaction temperature is controlled at 52±2°C. After toluene is cooled and filtered, the intermediate cyanoethyl caprolactam crude product is obtained, and its yield is 90%, (calculated by caprolactam), and the caprolactam conversion rate is 99%;

[0025] In a 2000ml four-necked bottle, add 600ml of distilled water, add 50g of the original four-component catalyst powder, start stirring and heat up to 90°C, and start to add sodium hydroxide solution dropwise. The initial concentration of sodium hydroxide solution is 10%, and a total of 310ml is added dropwise. 140ml of 25% sodium hydroxide solution was added dropwise, and the temperature was controlled at 88 ± 2 ° C. After all the sodium hydroxide solution was dripped, the temperature was raised to 94 ± 1 ° C a...

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Abstract

The invention relates to a process for preparing 1.8-dinitrogen bicyclo (5, 4, 0)-7-hendecene (DBU), which comprises, using aminocaprolactam and acrylic nitrile as initiation raw material, conducting addition reaction, hydrogenation reaction, polymerization reaction, hydrogenation catalysis.

Description

technical field [0001] The invention belongs to a method for preparing 1.8-diazabicyclo(5,4,0)-7undecene (hereinafter referred to as DBU). Background technique [0002] DBU is an amidine with a bi-heterocyclic structure, and is an important intermediate in organic synthesis. It can be widely used in various reactions such as elimination, isomerization, condensation, esterification, cyclization, and polymerization. The structural formula of DBU is: [0003] The relative molecular weight is 152.24, the boiling point is 259-260°C, and the density is 1.0192. It is a colorless or light yellow oily liquid. The preparation of DBU adopts the caprolactam method both at home and abroad, that is, using caprolactam and acrylonitrile as raw materials, and through three-step reactions of addition, hydrogenation and cyclization, the DBU product is prepared. The specific reaction process is as follows: [0004] <chemistry num="004"> <chem file="200310115849_cml001.xml" / > ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 马震马斌杨文库李全忠刘忠慧孙德彦
Owner 吉林省石油化工设计研究院