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Dimethylamine borane preparation method

A technology of dimethylamine borane and dimethylamine hydrochloride, applied in the field of compound preparation, can solve the problems of difficult control of reaction temperature, long reaction time, unsuitable for industrial production, etc., and achieves great application value, simple method and yield improved effect

Inactive Publication Date: 2012-10-10
SHANGHAI SHENYU PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method described in this patent is difficult to control the reaction temperature, and the reaction time is very long, so it is not suitable for industrial production

Method used

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  • Dimethylamine borane preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 81.55g (1mol) of dimethylamine hydrochloride and 150g of tetrahydrofuran into a 500ml reaction flask, and stir to mix. 37.83 g (1 mol) of sodium borohydride and 150 g of tetrahydrofuran were added to another reactor and stirred. Add dimethylamine hydrochloride / tetrahydrofuran dropwise to sodium borohydride / tetrahydrofuran, keep the internal temperature at 25-30°C, and stir for 4 hours. Then add 150g (25°C) saturated sodium chloride / 3% sodium hydroxide solution to the reaction system, stir at 25°C for 0.5 hour, stand still for 0.5 hour, and remove the lower layer solution. Add 10 g of sodium hydroxide to the upper layer solution, stir for 0.5 hour, stand still for 0.5 hour, and remove the lower alkaline aqueous layer. The supernatant was filtered and then distilled under normal pressure (25-85°C) and then under reduced pressure (0.09MPa, 25-85°C) to recover 250g of tetrahydrofuran. In the concentrated solution obtained after distillation, add 20g of 30% sodium hydr...

Embodiment 2

[0024] Add 81.55g (1mol) of dimethylamine hydrochloride and 150g of tetrahydrofuran into a 500ml reaction flask, and stir to mix. 53.83 g (1 mol) of potassium borohydride and 150 g of tetrahydrofuran were added to another reactor and stirred. Add dimethylamine hydrochloride / tetrahydrofuran dropwise to sodium borohydride / tetrahydrofuran, keep the internal temperature at 25-30°C, and stir for 4 hours. Then add 150g (25°C) saturated potassium chloride / 3% sodium hydroxide solution to the reaction system, stir at 25°C for 1 hour, stand still for 1 hour, and remove the lower layer solution. Add 10 g of sodium hydroxide to the upper layer solution, stir for 1 hour, stand still for 1 hour, and remove the lower alkali water layer. The supernatant was filtered and then distilled under normal pressure (25-85°C) and then under reduced pressure (0.09MPa, 25-85°C) to recover 250g of tetrahydrofuran. Add 20g of 30% sodium hydroxide solution to the concentrated solution obtained after disti...

Embodiment 3

[0026] With above-mentioned example 1, after adding sodium hydroxide solution to the concentrated solution after example 2 distillation, after directly adding the water of 9 times of solid weight amount, can be made into 10% dimethylamine borane aqueous solution.

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Abstract

The invention provides a dimethylamine borane preparation method. Sodium borohydride or potassium borohydride is reacted with dimethylamine hydrochloride in tetrahydrofuran solvent at the temperature ranging from 25 DEG C to 30 DEG C, the yield can reach 90%, and the purity is 99.5%. The unfavorable conditions that the reaction is difficult to control and reaction solvent is prone to volatilize when two solid reactants are added into one reaction bottle simultaneously are avoided by means of respective burdening and dripping reaction. Consumption of tetrahydrofuran serving as the reaction solvent is lowered by 50%, and using alkaline solution for separative purification after reaction is completed can reduce loss of inorganic salt adsorption feed liquid in a direct filtration method, improve yield and increase solvent recovery rate. Crystallization is directly performed under a solvent-free condition after treatment by the alkaline solution is completed. The dimethylamine borane preparation method is simple, convenient to operate, high in yield and product quality and suitable for industrial production and has high application value.

Description

technical field [0001] The invention relates to a compound preparation method, in particular to a preparation method of dimethylamine borane. Background technique [0002] Dimethylamine borane (DMAB) is a highly selective reducing agent for boron compounds in organic synthesis reactions. At present, it has been used in the electroplating industry, and is considered to be a new type of electroplating solution additive that can be used in a wide range of pH values, and it can be better miscible with a series of electroplating solutions. In the process of electroless nickel plating, a high-purity nickel film (Ni-B) alloy coating is formed on the surface of the plated part, which greatly enhances the brightness and hardness of the plated part surface, and also improves the heat resistance and electrical conductivity. and weldability. Other noble metals besides nickel are also suitable. Especially in the production process of electronic printed circuit boards, it has been wide...

Claims

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Application Information

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IPC IPC(8): C07F5/02C07F5/00
Inventor 郎中龄滕绍云厉文豪
Owner SHANGHAI SHENYU PHARMA & CHEM
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