Synthesis process of dimethylamine borane

A dimethylamine borane, synthesis process technology, applied in the preparation of amino compounds from amines, inorganic chemistry, metal hydrides, etc., can solve the problems of sacrificing reaction efficiency and reaction safety, and achieve the possibility of avoiding safety risks, Efficiency improvement and size reduction effect

Active Publication Date: 2018-09-28
广东乐远化学材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of sacrificing reaction efficiency and cost in exchange for reaction safety in the existing process,

Method used

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  • Synthesis process of dimethylamine borane
  • Synthesis process of dimethylamine borane
  • Synthesis process of dimethylamine borane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Continuously fill the 1000mL reaction flask with nitrogen to maintain the flow rate of nitrogen, add 30.7g (0.82mol) sodium borohydride and 100mL tetrahydrofuran into the reaction flask, control the temperature at 8±2°C, and add the dihydrofuran in 5 batches under vigorous stirring. Methylamine hydrochloride 55.3g (0.68mol), fully reacted for 1 to 2 hours; the obtained reaction solution was filtered, the filtrate was directly subjected to vacuum distillation, and then saturated sodium hydroxide solution was added to the concentrated solution obtained by distillation, and after stirring, Stand still, remove the lower alkali aqueous solution, and directly cool and crystallize the upper layer solution in a solvent-free state to obtain 40.8 g of dimethylamine borane as a solid, with a yield of 85% and a purity of 99%, as shown in batch 1 in the following table;

[0033] According to the same synthesis method as batch 1, the sodium borohydride / dimethylamine hydrochloride feed...

Embodiment 2

[0045] The solution of the present invention-industrial grade

[0046]Continuously fill the 5000mL reaction flask with nitrogen to maintain the flow rate of nitrogen, add 189.15g (5mol) sodium borohydride and 700mL tetrahydrofuran into the reaction flask, control the temperature at 8±2°C, and add dimethylformamide in 10 batches under vigorous stirring Amine hydrochloride 509.62g (6.25mol), fully reacted 5 hours; The obtained reaction solution was filtered, and the filtrate was directly subjected to vacuum distillation, then in the concentrated solution obtained by distillation, a saturated sodium hydroxide solution was added, stirred, and then separated Remove the lower alkali aqueous solution, and directly cool and crystallize the upper layer solution in a solvent-free state to obtain 259.25 g of dimethylamine borane as a solid, with a yield of 88% and a purity of 99%. See Batch 6 in the following table;

[0047] Control scheme - industrial grade

[0048] Add 189.15g (5mol) ...

Embodiment 3

[0052] The solution of the present invention-industrial grade

[0053] Fill the 5000mL reaction flask with nitrogen continuously to maintain the nitrogen flow rate, add 407.7g (5mol) dimethylamine hydrochloride and 1000mL tetrahydrofuran into the reaction flask, control the temperature at 8±2°C, and divide into 5 batches under vigorous stirring Add 151.32 g (4 mol) of sodium borohydride and react fully for 4 hours; filter the obtained reaction solution, and directly carry out vacuum distillation on the filtrate, then add saturated sodium hydroxide solution to the concentrated solution obtained by distillation, stand still after stirring, and separate The lower layer of alkali aqueous solution, the upper layer solution was directly cooled and crystallized in a solvent-free state, and 214.46 g of dimethylamine borane solid was obtained, with a yield of 91% and a purity of 99%. See batch 8 in the following table;

[0054] Control scheme - industrial grade

[0055] Add 407.7g (5m...

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Abstract

The invention discloses a synthesis process of dimethylamine borane. The process includes the steps of making hydroboron MBH4 and dimethylamine hydrochloride (CH3)2NH HCl mixed and sufficiently reacting in a solvent at the controlled temperature of 5-15 DEG C under the protection of inert gas to generate dimethylamine borane, and conducting after-treatment to remove the organic solvent and salt toobtain a water solution or solid of dimethylamine borane. The synthesis process is conducted under the reaction conditions of injecting inert gas for protection, hydrogen generated in reaction is brought away in time, safety risks are effectively reduced, the feeding speed and reaction severity can be tolerated to a large extent in the reaction, and the process has the advantages of being efficient, safe, capable of saving energy and the like on the premise of basically realizing the yield and purity in the prior art.

Description

technical field [0001] The invention relates to a synthesis process of dimethylamine borane, belonging to the technical field of chemical synthesis. Background technique [0002] Dimethylamine borane (DMAB) is a highly selective reducing agent commonly used in chemical synthesis. Due to its good pH compatibility and solubility, it is also more and more widely used in the electroplating industry, and the market demand is large. [0003] Existing DMAB preparation mainly utilizes dimethylamine hydrochloride and sodium borohydride or potassium borohydride to react in a solvent and obtain through purification, and the purity is about 85%~99.5%. The reaction formula of the synthesis process is: (CH 3 ) 2 NH·HCl+MBH 4 →(CH 3 ) 2 NH·BH 3 +MCl+H 2 . Because the reaction will generate a large amount of heat and generate hydrogen, the operation is dangerous and the controllability is poor in industrial production, so the requirements for the production process are relatively hig...

Claims

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Application Information

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IPC IPC(8): C07C211/04C07C209/68C01B6/13
CPCC01B6/13C07C209/68C07C211/04
Inventor 黄远彪
Owner 广东乐远化学材料科技有限公司
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