A preparing method of 1-ethyl-2-acetylpyrrole

A technology of acetylpyrrole and dimethylacetamide, which is applied in the field of preparation of N-ethyl-2-acetylpyrrole, can solve the problems of low content of finished products, low yield and the like, and achieves high content of finished products and easy availability of raw materials , The effect of simple and easy process operation

Active Publication Date: 2018-04-10
SHANDONG JITIAN AROMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The third is to synthesize N-ethyl-2-acetylpyrrole through 2-acetylpyrrole and iodoethane, with low yield and low content of finished product

Method used

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Experimental program
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Effect test

Embodiment 1

[0027] A preparation method of N-ethyl-2-acetylpyrrole, using pyrrole as a starting material, and preparing N-ethyl-2-acetylpyrrole through a two-step reaction operation, comprising the following steps:

[0028] 1. Preparation of 2-acetylpyrrole:

[0029] 1) Take a 1.1L three-necked flask, install a stirrer, a thermometer and a constant pressure dropping funnel, and place the lower part of the three-necked flask in a water bath to cool down;

[0030] 2) Add 25g (0.371mol) of pyrrole, 35g (0.402mol) of N,N-dimethylacetamide, and 250g of 1,2-dichloroethane into the three-necked flask, and stir well after adding;

[0031] 3) Control the temperature at 40±2°C, add 62g (0.405mol) of phosphorus oxychloride dropwise into the bottle, and add dropwise for 30 minutes;

[0032] 4) Keep warm at 40±2°C after dropping, and react for 2 hours;

[0033] 5) Pour the reaction solution into 200g crushed ice to freeze;

[0034] 6) Neutralize with 30% caustic soda solution to pH 7;

[0035] 7) ...

Embodiment 2

[0047] A preparation method of N-ethyl-2-acetylpyrrole, using pyrrole as a starting material, and preparing N-ethyl-2-acetylpyrrole through a two-step reaction operation, comprising the following steps:

[0048] 1. Preparation of 2-acetylpyrrole:

[0049] 1) Add 50kg (0.371mol) of pyrrole, 70kg (0.402mol) of N,N-dimethylacetamide, and 500kg of 1,2-dichloroethane into the reactor, and stir evenly after adding;

[0050] 2) Control the temperature at 40±2°C, add 124kg (0.405mol) of phosphorus oxychloride dropwise to the reaction kettle, and add dropwise for 30 minutes;

[0051] 3) Keep warm at 40±2°C after dropping, and react for 2 hours;

[0052] 4) Pour the reaction solution into 400kg crushed ice to freeze;

[0053] 5) Neutralize to pH 7 with 30% caustic soda solution;

[0054] 6) Extract with dichloroethane 200L×5, and concentrate the organic phase to 100°C under normal pressure to obtain the crude product;

[0055] 7) Recrystallize the obtained crude product with water t...

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Abstract

A preparing method of 1-ethyl-2-acetylpyrrole is disclosed. Pyrrole is adopted as an initial raw material and is subjected to two reaction steps to prepare the 1-ethyl-2-acetylpyrrole. Firstly, 2-acetylpyrrole is prepared from the pyrrole, N,N-dimethylacetamide, 1,2-dichloroethane and phosphorus oxychloride; and then the 1-ethyl-2-acetylpyrrole is prepared from KOH, water, trimethylstearylammoniumchloride, the 2-acetylpyrrole and diethyl carbonate. Beneficial effects of the method are that the method is safe and environment-friendly, a process is simple to operate and feasible, a finished product is high in content, raw materials are easily available, a production cost is low, and the method is suitable for large-scale production.

Description

Technical field: [0001] The invention specifically relates to a preparation method of N-ethyl-2-acetylpyrrole, which belongs to the technical field of chemical industry. Background technique: [0002] N-ethyl-2-acetylpyrrole, English name: N-Ethyl-2-Acetylpyrrole, Chinese alias: N-ethyl-2-acetylpyrrole, CAS number: 39741-41-8, molecular formula: C8H11NO, molecular weight: 137.179, used in food flavors such as coffee and fruit. The synthetic method of N-ethyl-2-acetylpyrrole traditionally has three kinds: a kind of method is N-ethylpyrrole acetylation, and N-ethylpyrrole raw material is not easy to obtain; Another kind of method is 2-acetylpyrrole and tertiary Potassium butoxide first generates pyrrole potassium salt in anhydrous system, and then condenses with ethyl bromide to obtain it. This process requires high equipment and operation. The third is to synthesize N-ethyl-2-acetylpyrrole through 2-acetylpyrrole and iodoethane, which has low yield and low content of finish...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/34
CPCC07D207/34
Inventor 杨亮杨位祥
Owner SHANDONG JITIAN AROMA CHEM CO LTD
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