Preparation process for lithium aluminum hydride-tetrahydrofuran solution

A technology of lithium aluminum hydride and tetrahydrofuran, which can be applied to various metal hydrides, dissolution, dissolution and other directions, can solve problems such as explosive decomposition, and achieve the effect of safe use

Inactive Publication Date: 2015-07-08
车荣睿
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Pure lithium aluminum hydride is relatively stable below 120°C

Method used

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  • Preparation process for lithium aluminum hydride-tetrahydrofuran solution
  • Preparation process for lithium aluminum hydride-tetrahydrofuran solution

Examples

Experimental program
Comparison scheme
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Embodiment 1-12

[0026] 1. Weigh each raw material according to the amount in Table 1;

[0027] The dosage of each raw material in the embodiment 1-12 of table 1

[0028]

[0029] Two, prepare lithium aluminum hydride-tetrahydrofuran solution according to the following steps:

[0030] (1) Material preparation

[0031] 1. Grind block lithium hydride in a ball mill to below 100 mesh, and set aside;

[0032] 2. Add aluminum trichloride to ether several times in an ice-water bath to make an ether solution of aluminum trichloride;

[0033] (2) Complexation reaction

[0034] In a 1000ml three-necked flask, install stirring, a constant pressure funnel and a straight condenser, add diethyl ether, add lithium hydride, start stirring and raise the temperature to 28°C with an electric heating mantle, slowly drop the aluminum trichloride diethyl ether solution from the constant pressure funnel Add it to the ether solution of lithium hydride, and the dropping time is about 6-10 hours. The dropping p...

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Abstract

The invention especially relates to a preparation process for a lithium aluminum hydride-tetrahydrofuran solution, which belongs to the field of preparation technology for chemical reagents. The preparation process is characterized by comprising the following steps: material preparation; complexation reaction; drying by distillation; and preparation of the lithium aluminum hydride-tetrahydrofuran solution. The preparation process has the following advantages: a reducing agent with extremely strong reduction capability is synthesized, and rapid development of organic synthesis technology, especially development of the pharmaceutical industry, can be effectively promoted; the lithium aluminum hydride-tetrahydrofuran solution is safe, simple and convenient to use; and finished lithium aluminum hydride-tetrahydrofuran solution products with different concentrations can be blended according to market demands so as to meet demands of different process conditions.

Description

technical field [0001] The invention belongs to the field of preparation technology of fine chemical products, and in particular relates to a preparation technology of lithium aluminum hydride-tetrahydrofuran solution. Background technique [0002] Lithium aluminum hydride is a complex aluminum hydride with the molecular formula LiAlH 4 , with a molecular weight of 37.95, this product is a white porous light powder, which will turn gray due to decomposition when placed for a long time. Lithium aluminum hydride, abbreviated as LAH, is a very strong reducing agent in organic synthesis, especially for the reduction of esters, carboxylic acids and amides. Its appearance has revolutionized organic synthesis. Pure lithium aluminum hydride is relatively stable below 120°C and in dry air, but it decomposes explosively when it meets water. Lithium aluminum hydride is soluble in ether solvents such as ether and tetrahydrofuran, with a specific gravity of 0.917. It decomposes into li...

Claims

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Application Information

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IPC IPC(8): B01F1/00B01F3/12C01B6/24
Inventor 车荣睿车瀛照庄英俊
Owner 车荣睿
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