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Formamide preparation method

A formamide and dimethylformamide technology, applied in the field of formamide preparation, can solve the problems of complex catalyst preparation process, easy catalyst deactivation, low reaction yield, etc., and achieve high controllability, conversion rate and selectivity High, simple reaction process effect

Active Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although there are many studies on the preparation methods of amides, there are some disadvantages: for example, the catalyst preparation process is complicated, the reaction time is long, the reaction yield is low, the environment is polluted, and the catalyst is easily deactivated after the reaction.

Method used

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Examples

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Effect test

Embodiment 1

[0024] In a 150ml pressure bottle, add 15mmol benzylamine and 20ml N,N-dimethylformamide respectively, and use CO 2 After gas replacement, the reaction was stirred at 100°C for 12 hours. After the reaction, the product was detected by chromatography. The conversion rate and selectivity are shown in Table 1.

Embodiment 2

[0026] In a 150ml polytetrafluoroethylene lined reactor, add 15mmol n-butylamine and 20ml formamide respectively, and charge CO 2 , The pressure is 0.6MPa. The reaction was stirred at 120°C for 12 hours. After the reaction, the product was detected by chromatography. The conversion rate and selectivity are shown in Table 1.

Embodiment 3

[0028] In a 150ml polytetrafluoroethylene-lined reactor, add 15mmol benzylamine and 20ml N,N-diethylformamide, and charge CO 2 , The pressure is 0.2MPa, and the reaction is stirred at 80°C for 24h. After the reaction is completed, the product is detected by chromatography. The conversion rate and selectivity are shown in Table 1.

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Abstract

The invention relates to a formamide preparation method. The method allows the product formamide to prepared from a formylating reagent and amine (primary amine or secondary amine) through a formylating reaction under the promotion of an acidic gas. The method is characterized in that the formylating reaction is efficiently carried out under mild conditions with the acidic gas as a reaction promoter. The method comprises the following steps: mixing a certain concentration of the formylating reagent with the primary amine or secondary amine without adding other solvents, introducing a certain amount of the acidic gas, sealing, stirring at a temperature higher than room temperature, and reacting for 0.5h or more to obtain the product formamide. The method has the advantages of high controllability and no addition of a catalyst in the reaction process; the promoter is a gas and rapidly volatilizes when the reaction ends, so separation is not needed; the yield of the product formamide reaches above 95%; and the promoter has very good substrate universality.

Description

Technical field [0001] The invention relates to a method for preparing formamide, in particular to a process for preparing formamide through a formamide reaction promoted by acid gas. Background technique [0002] Amide group is a very important chemical group that exists in many natural polymers, such as: peptides, proteins, etc. In addition, amide is also an excellent synthetic monomer and can be used to prepare polymers such as nylon. CN101970675A discloses a method for biocatalyzing nitrile compounds to prepare amide compounds. A patent of BASF Europe (CN102712576A) uses phosphoric acid or Lewis acidic metal salt as a catalyst to catalyze the conversion of a series of amines and formate esters to prepare aromatic formamides. Patent CN101684076B uses amino acid ionic liquid as reaction medium and catalyst to catalyze the Beckmann rearrangement reaction of ketoxime to prepare amide. [0003] Although there are many studies on the preparation methods of amides, there are some d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B43/06C07C231/10C07C231/02C07C233/03C07C233/18C07C233/13C07D307/52C07D333/20
Inventor 王峰王业红徐杰张健张晓辰张超锋陈海军
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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