Sodium tert-butoxide preparation process

A sodium tert-butoxide and preparation technology, applied in the field of compound synthesis, can solve the problems of reducing the reaction contact area, increasing the risk factor, and long time, so as to facilitate safe production, increase the contact area, and simplify the preparation process Effect

Inactive Publication Date: 2019-04-05
南京大地药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this method is: 1, metal sodium must be cut into pieces, and the whole process is preferably protected with nitrogen; 2, it takes a long time to add sodium flakes in the reactor, which increases the chance of the reaction system contacting with air, The risk factor increases; 3. The boiling point of tert-butanol is 82°C, and metal sodium will not dissolve in it, so the sodium flakes are easy to gather. In this way, the reaction contact area is reduced, and the stirring force of the reactor is increased. load

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:

[0028] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.04%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;

[0029] (2) Add 23g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;

[0030] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated duri...

Embodiment 2

[0033] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:

[0034] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.04%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;

[0035] (2) Add 25.56g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;

[0036] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated d...

Embodiment 3

[0039] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:

[0040] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.03%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;

[0041] (2) Add 27.6g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;

[0042] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated du...

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PUM

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Abstract

The invention discloses a sodium tert-butoxide preparation process. The process includes steps: (1) taking o-xylene as a solvent of a reaction system, adding into a reaction kettle, and adding sodiumblocks into the reaction kettle to melt to obtain a reactant; (2) heating the reaction kettle, adding tert-butyl alcohol, and performing reaction to obtain a crude product of sodium tert-butoxide; (3)subjecting the crude product of sodium tert-butoxide to aftertreatment to obtain a finished product of sodium tert-butoxide. The preparation process has advantages that slicing metal sodium before reaction is avoided, so that a preparation process is simplified, and reaction is facilitated due to increasing of reaction contact area.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a preparation process of sodium tert-butoxide. Background technique [0002] Sodium tert-butoxide, also known as sodium tert-butoxide, English name Sodium tert-butoxide, white crystal, molecular formula C 4 h 9 NaO, with a molecular weight of 96.10, is stable at normal temperature and pressure, and is slightly harmful to water. It is used as an intermediate in organic synthesis and pharmaceutical intermediates; or as a strong base, it is widely used in the condensation of chemical, pharmaceutical, pesticide and organic synthesis. , rearrangement and ring-opening reactions, therefore, sodium tert-butoxide is more and more favored by the fine chemical industry, pesticide and pharmaceutical industries. [0003] The traditional preparation process of sodium tert-butoxide generally uses tert-butanol as the reaction solvent directly, and then slowly puts the pre-cut piec...

Claims

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Application Information

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IPC IPC(8): C07C29/70C07C31/30
CPCC07C29/70C07C31/30
Inventor 唐景彪孔晓明
Owner 南京大地药业有限公司
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