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Preparation method of tri(dimethylamino)borane

A technology of dimethylamino and borane, applied in the field of preparation, can solve the problems of high toxicity, difficult transportation and storage, etc.

Inactive Publication Date: 2013-04-03
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problems in the prior art of preparing tris(dimethylamino)borane from highly toxic dimethylamine and its organic solvent solution, which is highly toxic and difficult to transport and store, and provides three The preparation method of (dimethylamino) borane

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  • Preparation method of tri(dimethylamino)borane

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specific Embodiment approach 1

[0016] Specific embodiment one: the preparation method of tris(dimethylamino)borane in this embodiment is specifically prepared according to the following steps:

[0017] 1. According to the material ratio of boron trihalide, dimethylamine salt and alkali as 1:6~12:6~18, weigh the organic solution of boron trihalide and dimethylamine with a mass concentration of 15%~30%. Salt and alkali solution with mass concentration of 30%~60%;

[0018] 2. Add the alkali solution weighed in step 1 into the dimethylamine salt at room temperature under stirring conditions to obtain dimethylamine gas, and control the stirring speed to 50r / min~800r / min;

[0019] Three, the dimethylamine gas that step 2 obtains is passed through potassium hydroxide drier, obtains the dimethylamine gas of drying;

[0020] 4. At a temperature of -20°C~5°C, pass dry dimethylamine gas into the continuously stirring boron trihalide organic solution, then continue stirring for 1h~1.5h, and control the stirring speed ...

specific Embodiment approach 2

[0024] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that the ratio of boron trihalide, dimethylamine salt and alkali in step 1 is 1:7~10:9~15. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0025] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that: the mass concentration of the boron trihalide organic solution in step 1 is 18%-25%. Others are the same as in the first or second embodiment.

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Abstract

The invention provides a preparation method of tri(dimethylamino)borane, relating to a preparation method. The invention aims to solve the problems of large toxicity and difficulty in transportation and storage when the tri(dimethylamino)borane is prepared by adopting dimethylamine with large toxicity and an organic solvent solution of the dimethylamine in the prior art. The preparation method comprises the steps of: 1, weighing; 2, obtaining a dimethylamine gas; 3, drying; 4, obtaining a solid-liquid mixture; and 5, filtering and collecting. According to the invention, the dimethylamine and an organic solvent solution of the dimethylamine are not used, thus the problems of large toxicity and difficulty in transportation and storage of the dimethylamine as a reaction raw material are solved; and a filter cake obtained in an intermediate process can be used as a raw material for being recycled. The preparation method is used for preparing the tri(dimethylamino)borane.

Description

technical field [0001] The invention relates to a preparation method. Background technique [0002] Tris(dimethylamino)borane is an intermediate in the synthesis of bis-pinacol diborane. The synthetic route of tris(dimethylamino)borane is to add a solution of boron trihalide (boron tribromide or boron trichloride) dropwise into a solution of dimethylamine. The solvent can be n-pentane, petroleum ether, sulfolane, etc. Documents (Org.Synth.2000,77,176~180; J.Am.Chem.Soc.1960,82,6242~6245) mentioned that the n-pentane solution of boron tribromide was added dropwise to dimethylamine at low temperature of n-pentane solution, and filtered to obtain tris(dimethylamino)borane. It is mentioned in the patent (CN200710010757) that sulfolane is used as a solvent, and petroleum ether (40-60) is used as a solvent in the literature (J.Org.Chem.1981, 46, 1309~1314), and dimethylamine is directly used in the above literature Or use an organic solution of dimethylamine. [0003] However...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 李猛李淑辉张惠白雪峰胡永玲宁志强徐虹
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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