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Cost-saving preparation method of p-nitrobenzyl alcohol

A cost-saving technology for p-nitrobenzyl alcohol, which is applied in the field of synthesis technology of p-nitrobenzyl alcohol, and achieves the effects of low preparation cost, simple process and simple reaction system

Inactive Publication Date: 2015-02-25
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem solved by the present invention is to provide a kind of preparation method of p-nitrobenzyl alcohol which is simple and easy to operate, cheap and easy to obtain raw materials, high in reaction efficiency and good in repeatability, and cost-saving. The method is used to prepare p-nitrobenzyl alcohol Alcohol overcomes the shortcomings of high raw material price and low yield, and can obtain considerable commercial value

Method used

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  • Cost-saving preparation method of p-nitrobenzyl alcohol
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  • Cost-saving preparation method of p-nitrobenzyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of p-nitrobenzyl chloride

[0019] Take 1mol of p-nitrotoluene, 5mmol of benzoyl peroxide, and 1mol of carbon tetrachloride into the reaction flask, heat to 150°C and reflux at a stirring speed of 250-500r / min, and introduce chlorine gas, and the time is controlled at 1- 2h; after adding, continuously sample during the reaction and carry out chromatographic analysis. When the yield of p-nitrobenzyl chloride reaches about 50%, the raw material p-nitrotoluene is distilled out at 180° C. The total yield of nitrobenzyl chloride is increased to 88%. At the same time, the hydrogen chloride gas generated during the reaction is discharged to the tail gas absorption system to be absorbed into hydrochloric acid by water. Finally, the crude product of nitrobenzyl chloride is crystallized with 3mol absolute ethanol as a solvent Purification, the product with a purity higher than 99.0% can be obtained.

Embodiment 2

[0021] Preparation of p-nitrobenzyl chloride

[0022] Take 1mol of p-nitrotoluene, 4mmol of benzoyl peroxide, and 1.2mol of carbon tetrachloride into the reaction flask, heat to 160°C and reflux at a stirring speed of 250-500r / min, and feed in chlorine gas for a time of 1 -2h; After adding, keep sampling during the reaction and carry out chromatographic analysis. When the yield of p-nitrobenzyl chloride reaches about 37%, the raw material p-nitrotoluene is distilled out at 190°C and chlorinated again. Repeat the above steps to make The total yield of p-nitrobenzyl chloride is increased to 89%. At the same time, the hydrogen chloride gas produced in the reaction process is discharged to the tail gas absorption system to be absorbed into hydrochloric acid with water, and finally the crude product of p-nitrobenzyl chloride is used as a solvent with 3mol absolute ethanol Crystallization and purification can obtain products with a purity higher than 98.0%.

Embodiment 3

[0024] Preparation of p-nitrobenzyl chloride

[0025] Take 1mol of p-nitrotoluene, 6mmol of benzoyl peroxide, and 1.3mol of carbon tetrachloride into the reaction flask, heat to 150°C and reflux at a stirring speed of 250-500r / min, feed chlorine gas, and control the time at 1 -2h; After the addition, the reaction is continuously sampled for chromatographic analysis. When the yield of p-nitrobenzyl chloride reaches about 40%, the raw material p-nitrotoluene is distilled out by steam distillation at 100°C and then chlorinated again. Repeat the above steps to make The total yield of p-nitrobenzyl chloride is increased to 86%. At the same time, the hydrogen chloride gas produced in the reaction process is discharged to the tail gas absorption system to be absorbed into hydrochloric acid with water. Finally, the crude product of p-nitrobenzyl chloride is used as a solvent with 3mol absolute ethanol Crystallization and purification can obtain products with a purity higher than 99.0%...

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Abstract

The invention discloses a cost-saving preparation method of p-nitrobenzyl alcohol. The key points of the technical scheme are as follows: according to the cost-saving preparation method of the p-nitrobenzyl alcohol, p-nitrotoluene is taken as a starting raw material and reacts with chlorine gas to obtain p-nitrobenzyl chloride, and then the p-nitrobenzyl chloride is hydrolyzed in an alkaline solution to obtain p-nitrobenzyl alcohol. Compared with the prior art, the cost-saving preparation method of the p-nitrobenzyl alcohol has the following beneficial effects: the reaction system is simple and the raw material is cheap and easily available; the preparation cost is low and no hazardous waste is generated, so that the preparation method accords with the green production ideal; the cost-saving preparation method is simple in process, simple and convenient to operate, short in reaction time, high in efficiency and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of synthesis technology of p-nitrobenzyl alcohol, and in particular relates to a cost-saving preparation method of p-nitrobenzyl alcohol. Background technique [0002] p-nitrobenzyl alcohol, also known as 4-nitrobenzyl alcohol or p-nitrobenzyl alcohol, is a white or light yellow crystal with a melting point of 92-94°C and a boiling point of 185°C (12mmHg). It is easily soluble in solvents and soluble in water. It is mainly used as a protective group in the synthesis of antibiotics, a pharmaceutical intermediate and a raw material for general organic synthesis. Its derivatives can inhibit the activity of trypsin and can be used to treat tumors. The current technique of synthesizing p-nitrobenzyl alcohol has the disadvantages of high raw material price and low yield. [0003] The preparation method of reported p-nitrobenzyl alcohol mainly contains reduction method and hydrolysis method, and the former compris...

Claims

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Application Information

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IPC IPC(8): C07C205/19C07C201/12
Inventor 陈得军李凌君朱安莲裴渊超
Owner HENAN NORMAL UNIV
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