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A formamide and secondary amine technology, applied in the field of formamide preparation, can solve the problems of environmental pollution, complex catalyst preparation process, and low reaction yield
Active Publication Date: 2015-03-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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[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.
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Embodiment 1
[0028] CeO obtained by roasting method 2 The process is as follows: directly roast cerium ammonium nitrate at 650°C for 2 hours, and the obtained CeO 2 , denoted as CEO-1, applied to the reaction of benzylamine with N,N-dimethylformamide. In a 150ml Teflon-lined reactor, add 15mmol benzylamine and 20ml N,N-dimethylformamide respectively, weigh 1g CEO-1 to catalyze the reaction, stir the reaction at 100°C for 12h, after the reaction , the chromatographic detection product, its conversion rate and selectivity are shown in Table 1.
Embodiment 2
[0030] CeO obtained by co-precipitation method 2 The process is as follows: dissolve cerium nitrate in water, adjust the pH to 11 with ammonia water, filter and separate, dry the filter cake at 100°C overnight, and roast at 500°C for 4 hours to obtain CeO 2 Denoted as CEO-2, it is used in the hydrolysis reaction of benzylamine and N,N-dimethylformamide. In a 150ml Teflon-lined reactor, add 15mmol benzylamine and 20ml N,N-dimethylformamide respectively, weigh 1g CEO-2 to catalyze the reaction, stir the reaction at 100°C for 12h, after the reaction , the chromatographic detection product, its conversion rate and selectivity are shown in Table 1.
Embodiment 3
[0032] Dissolve cerium ammonium nitrate and polyvinylpyrrolidone in ethylene glycol, reflux at 190°C for 24 hours, filter and separate, vacuum-dry the filter cake at 80°C, and roast at 600°C to obtain CeO 2 Denoted as CEO-3, it is used in the hydrolysis reaction of benzylamine and N,N-dimethylformamide. In a 150ml Teflon-lined reactor, add 15mmol benzylamine and 20ml N,N-dimethylformamide respectively, weigh 1g CEO-3 to catalyze the reaction, stir the reaction at 100°C for 12h, after the reaction , the chromatographic detection product, its conversion rate and selectivity are shown in Table 1.
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Abstract
The invention relates to a preparation method of methanamide. The method uses formamide or its derivative and amine (primary or secondary amine) as reactants, which are subjected to amidomethylation in the presence of a catalyst to prepare methanamide. The method is characterized in that solid acidic metal oxide or precious metal loaded acidic metal oxide is used as the catalyst and the reaction is carried out efficiently under mild conditions. The reaction process is as follows: mixing formamide with certain concentration or its derivatives with primary or secondary amine and a certain amount of catalyst, placing the mixture into pressure vessel without adding or additionally adding other solvent, sealing, stirring at a temperature no less than 60 DEG C, and reacting for no less than 0.5 h to obtain the reaction product methanamide. The method has the advantages of simple preparation of the catalyst, easy separation process of the catalyst and product, repeated usage of the catalyst, high controllability of the reaction process, and yield of the product formamide reaching more than 95%.
Description
technical field [0001] The invention relates to a method for preparing formamide, in particular to catalyzing the formamide reaction of formamide or its derivatives with amines (primary or secondary amines) to prepare formamide as a product. Background technique [0002] The amide group is a very important chemical group that exists in many natural polymers, such as: polypeptides, proteins, etc. In addition, amides are also excellent synthetic monomers, which can be used to prepare polymers such as nylon. CN101970675A discloses a method for preparing amide compounds by biocatalyzing nitrile compounds. A patent (CN102712576A) of BASF Europe uses phosphoric acid or Lewis acidic metal salts as catalysts to catalyze the conversion of aromatic amines and formates 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 amides. [0003] Although there a...
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