Fluorine-containing amide and preparation method thereof

A technology containing fluorine-containing amides and dimethylethylenediamine, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds. The effect of short operation and process cycle and simple reaction steps

Inactive Publication Date: 2019-01-18
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods use highly toxic anhydrous hydrogen fluoride, fluorine gas or highly volatile fluorides as fluorinating agents, which will cause imme

Method used

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  • Fluorine-containing amide and preparation method thereof
  • Fluorine-containing amide and preparation method thereof
  • Fluorine-containing amide and preparation method thereof

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[0023] The present invention will be further described in detail below with reference to the drawings and specific steps. The present invention discloses a fluorine-containing amide and a preparation method thereof. The preparation method specifically includes the following steps:

[0024] Step 1. Take N,N-dimethylethylenediamine and add it to distilled water, the mixing ratio is 3mol: 2L, and obtain N,N-dimethylethylenediamine aqueous solution after thorough stirring;

[0025] Step 2. Take ethyl trifluoroacetate equimolar with N,N-dimethylethylenediamine and slowly add it dropwise to the N,N-dimethylethylenediamine aqueous solution using a constant pressure dropping funnel. The dropping time is 0.5~1h to obtain the reaction system;

[0026] Step 3. The reaction system obtained in step 2 is reacted at 0 to 30°C for 2 to 4 hours, and solution A is obtained after the reaction is completed;

[0027] In step 4, the solution A is distilled under reduced pressure and freeze-dried to obtain ...

Example Embodiment

[0033] Example 1

[0034] Step 1. Take 0.03 mol of N,N-dimethylethylenediamine and add it to 0.02L of distilled water, and stir thoroughly to obtain an aqueous solution of N,N-dimethylethylenediamine;

[0035] Step 2. Take 0.03 mol of ethyl trifluoroacetate and slowly add it dropwise to the N,N-dimethylethylenediamine aqueous solution using a constant pressure dropping funnel for 0.5h to obtain a reaction system;

[0036] Step 3. The reaction system obtained in step 2 was reacted at 10°C for 3 hours, and solution A was obtained after the reaction was completed;

[0037] In step 4, the solution A is distilled under reduced pressure and freeze-dried to obtain yellow crystals, namely N-[2-(dimethylamino)ethyl]-2,2,2-trifluoroacetamide.

Example Embodiment

[0038] Example 2

[0039] Step 1. Take 3 mol of N,N-dimethylethylenediamine and add it to 2L of distilled water, and stir thoroughly to obtain an aqueous solution of N,N-dimethylethylenediamine;

[0040] Step 2. Take 3 mol of ethyl trifluoroacetate and slowly drop it into the N,N-dimethylethylenediamine aqueous solution using a constant pressure dropping funnel for 1 hour to obtain a reaction system;

[0041] Step 3. The reaction system obtained in step 2 was reacted at 30°C for 2 hours, and solution A was obtained after the reaction was completed;

[0042] Step 4: Distill the solution A under reduced pressure and freeze-dry to obtain yellow crystals, namely N-[2-(dimethylamino)ethyl]-2,2,2-trifluoroacetamide.

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Abstract

The invention discloses fluorine-containing amide and a preparation method thereof. The method comprises the following step: taking an aliphatic fluorine-containing intermediate ethyl trifluoroacetateand N,N-dimethylethylenediamine to make acylation reaction, so as to obtain the fluorine-containing amide. The ethyl trifluoroacetate and the N,N-dimethylethylenediamine are used as raw materials andwater is used as a solvent; the acylation reaction is carried out to generate the fluorine-containing amide; the preparation method has the advantages of simple reaction steps, short technology period, easiness for operation, low reaction temperature and easy-to-control process; the yield of the fluorine-containing amide prepared by the method can reach 99 percent.

Description

【Technical field】 [0001] The invention belongs to the field of fine chemicals, and in particular relates to a fluorine-containing amide and a preparation method thereof. 【Background technique】 [0002] Fluorine-containing compounds have extraordinary effects and excellent properties. Therefore, the chemical industry in all countries in the world attaches great importance to fluorine-containing compounds. Due to the characteristics of the fluorine atom itself - small radius, high electronegativity, not easy to polarize, etc., fluorine-containing organic compounds have unique properties in terms of physics, chemistry and biology. The bond energy of the C-F bond formed by the fluorine atom and the carbon atom is much larger than the bond energy of the C-H bond formed by the hydrogen atom, so the organic fluorine compound usually has high thermal stability and chemical stability, and the physiological activity is also significant. Increase. In addition, fluorine-containing org...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/36
CPCC07C231/02C07C233/36
Inventor 郭睿刘雪艳霍文生李秀环冯文佩高弯弯
Owner SHAANXI UNIV OF SCI & TECH
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