Synthesis method of borane-solvent complex

A synthesis method and borane technology, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of high risk, high toxicity, explosion, etc., and achieve convenient operation, low cost and low toxicity. Effect

Inactive Publication Date: 2016-10-05
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

However, both boron trifluoride and boron trichloride are very toxic, and will explode wh

Method used

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  • Synthesis method of borane-solvent complex
  • Synthesis method of borane-solvent complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The operation steps are described as follows:

[0028] 1) Weigh 11.4237g of sodium borohydride and dissolve it in 300ml of tetrahydrofuran.

[0029] 2) Weigh 41.7182 g of lead chloride, and add it into a tetrahydrofuran solution of sodium borohydride.

[0030] 3) Stir the solution at room temperature.

[0031] 4) Until the sodium borohydride is completely consumed.

[0032] The reaction equation is: 2NaBH 4 +2THF+PbCl 2 =2NaCl+Pb+2THF·BH 3 +H 2

[0033] 5) Rotary evaporation, in the way of collecting in the cold trap, the borane tetrahydrofuran complex is separated from the precipitate.

[0034] 6) The solution collected in the cold trap is the borane tetrahydrofuran complex.

Embodiment 2

[0036] The operation steps are described as follows:

[0037] 1) Weigh 16.2333g of potassium borohydride and dissolve it in 300ml of tetrahydrofuran.

[0038] 2) Weigh 26.6975 g of bismuth trifluoride, and add it into a tetrahydrofuran solution of potassium borohydride.

[0039] 3) Stir the solution at room temperature.

[0040] 4) Until potassium borohydride is completely consumed.

[0041] The reaction equation is: 6KBH 4 +6THF+2BiF 3 =6KF+2Bi+6THF·BH 3 +3H 2

[0042] 5) Rotary evaporation, in the way of collecting in the cold trap, the borane tetrahydrofuran complex is separated from the precipitate.

[0043] 6) The solution collected in the cold trap is the borane tetrahydrofuran complex.

Embodiment 3

[0045] 1) Weigh 11.4812g of sodium borohydride and dissolve it in 300ml of tetrahydrofuran.

[0046] 2) Weigh 29.7753 g of cuprous chloride, and add it to a tetrahydrofuran solution of sodium borohydride.

[0047] 3) Stir the solution at room temperature.

[0048] 4) Until the sodium borohydride is completely consumed.

[0049] The reaction equation is: 2NaBH 4 +2THF+2CuCl=2NaCl+2Cu+2THF·BH 3 +H 2

[0050] 5) Centrifuge the solution at high speed.

[0051] 6) The collected supernatant is the borane tetrahydrofuran complex.

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Abstract

The invention relates to the field of borane solvent complex, and specifically relates to a synthesis method of a borane-solvent complex. According to the invention, a borohydride is dissolved in an organic solvent with a complexing function; metal inorganic salt is added, and stirring is carried out under a certain temperature, until the borohydride is completely consumed; and purification is carried out, such that the borane-solvent complex is obtained. The adopted reactants are borohydride and metal, and the reaction solvent is a solvent with a complexing function. With the method, the cost is low; reactant toxicity is low; and operation is convenient, simple and fast. The method is suitable for laboratory on-site preparation, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of borane solvent complexes, and in particular relates to a synthesis method of borane-solvent complexes. Background technique [0002] The complex of borane and solvent is the existing form after diborane is dissolved in solvent, and is a very useful reducing agent, usually the solvent complex of borane, such as borane tetrahydrofuran complex, its Preparation method: sodium borohydride and boron trifluoride (or boron trichloride) ether complex reaction in THF. However, both boron trifluoride and boron trichloride are very toxic, and will explode when exposed to water, which is highly dangerous. It is very unfavorable for experimental operation. [0003] The invention provides a simple and efficient synthesis method for borane, a widely used reducing agent, and the complex compound of borane and solvent synthesized by the invention can be directly used in various reduction reactions. Contents of the invention [...

Claims

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Application Information

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IPC IPC(8): C01B6/10
Inventor 陈萍陈维东黄振国
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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