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A kind of preparation method of n-ethyl-2-acetylpyrrole

A technology of acetylpyrrole and ethyl, which is applied in the field of preparation of N-ethyl-2-acetylpyrrole, can solve the problems of low finished product content and low yield, and achieve high finished product content, easy access to raw materials, and process operation simple and easy effects

Active Publication Date: 2021-05-11
SHANDONG JITIAN AROMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The third is to synthesize N-ethyl-2-acetylpyrrole by 2-acetylpyrrole and iodoethane, the yield is low, and the finished product content is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of preparation method of N-ethyl-2-acetylpyrrole, take pyrrole as starting material, make N-ethyl-2-acetylpyrrole through two-step reaction operation, comprise 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 evenly 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) Extrac...

Embodiment 2

[0047] A kind of preparation method of N-ethyl-2-acetylpyrrole, take pyrrole as starting material, make N-ethyl-2-acetylpyrrole through two-step reaction operation, comprise 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 to obtain...

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Abstract

The invention discloses a preparation method of N-ethyl-2-acetylpyrrole. Taking pyrrole as a starting material, N-ethyl-2-acetylpyrrole is prepared through a two-step reaction operation. Firstly, pyrrole, N , N-dimethylacetamide, 1,2-dichloroethane and phosphorus oxychloride to prepare 2-acetylpyrrole; then KOH, water, octadecyltrimethylammonium chloride, 2-acetyl N-ethyl-2-acetylpyrrole can be prepared from base pyrrole and diethyl carbonate. The beneficial effects of the invention are: safety and environmental protection, simple and easy process operation, high content of finished products, easily available raw materials, low production cost, and 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 by 2-acetylpyrrole and iodoethane, with low yield and low finished product content. C...

Claims

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Application Information

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Patent Type & Authority Patents(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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