Sodium tert-butoxide and preparation method thereof

A technology of sodium tert-butoxide and tert-butanol, which is applied in the field of compound synthesis, can solve the problems of not reaching the melting temperature of metal sodium, increasing the stirring load of the reactor, and increasing the danger of the production process, etc., and achieves the improvement of reaction speed, Improve production efficiency and be conducive to the effect of safe production

Inactive Publication Date: 2019-04-26
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

However, this method has the following disadvantages: 1. Sodium metal is easily oxidized by oxygen in the air, and nitrogen protection is required during the slicing process; 2. The boiling point of tert-butanol does not reach the melting temperature of sodium metal, so the sodium flakes are easy to gather , thereby reducing the reaction contact area and indirectly increasing the stirring load of the reactor
However, this method will release hydrogen gas during the reaction, which increases the danger of the production process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:

[0028] (1) Add 240 mL of heptane with a water content of 0.03% to the reactor, and then add sodium amide and tert-butanol with a molar mass ratio of 1:1.015, wherein the amount of sodium amide added is 9.8 g, and the amount of tert-butanol The amount of addition is 19g, stir well to make it dissolve completely, and obtain a mixed solution;

[0029] (2) The temperature of the mixed solution was raised to 70°C, and the reaction was carried out, and the ammonia gas released during the reaction was absorbed with water, and the heating was stopped after 2 hours of reaction to obtain the crude sodium tert-butoxide;

[0030] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under re...

Embodiment 2

[0032] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:

[0033] (1) Add 240 mL of heptane with a water content of 0.02% to the reactor, and then add sodium amide and tert-butanol with a molar mass ratio of 1:1.015, wherein the amount of sodium amide added is 0.25 mol, and the amount of tert-butanol The addition amount is 0.254mol, stir well to make it dissolve completely, and obtain a mixed solution;

[0034] (2) The temperature of the mixed solution was raised to 80°C, and the reaction was carried out. The ammonia gas released during the reaction was absorbed by lye, and the heating was stopped after 1.8 hours of reaction to obtain the crude sodium tert-butoxide;

[0035] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under red...

Embodiment 3

[0037] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:

[0038] (1) Add 240 mL of heptane with a water content of 0.01% to the reaction kettle, then add sodium amide and tert-butanol with a molar mass ratio of 1.015:1, stir thoroughly to dissolve completely, and obtain a mixed solution;

[0039] (2) The temperature of the mixed solution was raised to 100°C, and the reaction was carried out, and the ammonia gas released during the reaction was absorbed with water, and the heating was stopped after 1 hour of reaction to obtain the crude sodium tert-butoxide;

[0040] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under reduced pressure to obtain 23.8 g of white solid Powder, the product content is 99.2% through acid-base titration...

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Abstract

The invention discloses sodium tert-butoxide and a preparation method thereof. The preparation method comprises the following steps: (1) taking methylbenzene or heptanes as a reaction medium, adding sodium amide and tertiary butanol, mixing and stirring to dissolve to obtain a mixed solution; (2) heating the mixed solution to 70-110 DEG C for reaction to obtain a crude product of sodium tert-butoxide till the reaction is completed; (3) rectifying the crude product of the sodium tert-butoxide to obtain a finished product of the sodium tert-butoxide. The preparation method disclosed by the invention has relaxed reaction conditions, is small in danger in the production process, simple in aftertreatment process of products and short in drying time, and the product yield is up to 99% or above.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to sodium tert-butoxide and a preparation method thereof. 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. The traditional synthesis method of sodium tert-butoxide is to use tert-butanol directly as a solvent, and then slowly drop the pre-cut pieces of sodium metal into tert-butanol. After the reaction is completed, tert-butanol is distilled off to obtain sodium tert-butoxide. However, this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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