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Process for preparing triphenylchloromethane

A triphenylchloromethane, process technology, applied in the field of preparation of triphenylchloromethane, to achieve the effect of improving recycling, avoiding pollution problems, and good solubility

Pending Publication Date: 2021-06-18
江西华飞医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a process for preparing triphenylchloromethane, which not only improves the yield and purity of triphenylchloromethane, but also avoids pollution in the process The problem

Method used

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  • Process for preparing triphenylchloromethane
  • Process for preparing triphenylchloromethane
  • Process for preparing triphenylchloromethane

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Put 130g of pure benzene and 25g of anhydrous aluminum trichloride into a 250mL four-neck flask, control the temperature of the water bath at 25°C, slowly add carbon tetrachloride dropwise for 4 hours; Continue to raise the temperature to 78°C, carry out the reflux reaction for 3 hours, then lower the temperature to 25°C, keep the temperature for 30 minutes, and obtain the Friedel-Crafts reaction solution for later use, and collect the HCl gas generated during the process;

[0044] Put 88g of pure benzene and 150g of 15% hydrochloric acid aqueous solution into a 500mL four-neck flask. The temperature of the water bath is controlled at 10°C. Add the Friedel-Crafts reaction solution dropwise to the reaction flask for 0.5h, and continue to stir for 10min after the dropwise addition is completed. , stop stirring, separate layers after standing for 30min, remove the water layer, and wash the oil phase twice with 150g of 15% hydrochloric acid aqueous solution;

[0045] Collec...

Embodiment 2

[0049] Put 135g of pure benzene and 28g of anhydrous aluminum trichloride into a 250mL four-neck flask, control the temperature of the water bath at 30°C, slowly add carbon tetrachloride dropwise for 3.5h; after the addition of carbon tetrachloride, keep it warm for 2h Then continue to heat up to 70°C, carry out the reflux reaction for 3 hours, then lower the temperature to 25°C, keep it warm for 30 minutes, and obtain the Friedel-Crafts reaction solution for later use, and collect the HCl gas generated during the process;

[0050] Put 88g of pure benzene and 150g of 25% hydrochloric acid aqueous solution into a 500mL four-necked flask. The temperature of the water bath is controlled at 10°C. Add the Friedel-Crafts reaction solution dropwise to the reaction flask for 0.5h. After the dropwise addition, continue to stir for 10min. , stop stirring, separate layers after standing for 30min, remove the water layer, and wash the oil phase twice with 150g of 25% hydrochloric acid aque...

Embodiment 3

[0055] Put 265g of pure benzene and 60g of anhydrous aluminum trichloride into a 500mL four-neck flask, control the temperature of the water bath at 35°C, and slowly add carbon tetrachloride dropwise for 3.5h. After the carbon tetrachloride was added dropwise, keep warm for 2 hours and continue to heat up to 80°C. After reflux reaction for 3 hours, the temperature drops to 25°C. Keep warm for 30 minutes to get Friedel-Crafts reaction solution for later use; wherein, the HCl gas generated during the process is collected.

[0056] Put 160g of pure benzene and 350g of 20% hydrochloric acid aqueous solution into a 1000mL four-neck flask, control the temperature of the water bath at 10°C, add the spare material for Friedel-Crafts reaction to the reaction flask dropwise, the dropwise addition time is 0.5h, and continue to stir after the dropwise addition is completed After 10 minutes, stop stirring, let stand for 30 minutes, separate layers, remove the water layer, and wash the oil p...

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Abstract

The invention discloses a process for preparing triphenylchloromethane, which comprises the following steps of carrying out Friedel-Crafts reaction on pure benzene and carbon tetrachloride under the catalytic action of anhydrous aluminum trichloride to obtain a product containing Friedel-Crafts reaction liquid, dropwise adding the Friedel-Crafts reaction solution into a pure benzene and hydrochloric acid aqueous solution for quenching reaction, and standing for layering after dropwise adding to obtain an oil phase, introducing dry HCl gas and adding anhydrous calcium chloride into the oil phase, carrying out heat preservation reaction in a temperature environment, and then carrying out filter pressing to obtain an organic phase, carrying out atmospheric distillation on the organic phase, and continuing vacuum drying when no fraction exists to obtain a dry crude product, and adding a xylene solvent into the dried crude product for dissolving, adding anhydrous calcium chloride, introducing dry HCl gas, carrying out a heat preservation reaction in a temperature environment, removing the HCl gas and part of the xylene solvent after the reaction is finished, and carrying out hot filtration, freezing crystallization, filter pressing, washing and drying to obtain the product. The method not only improves the yield and purity of triphenylchloromethane, but also avoids the problem of pollution in the process.

Description

technical field [0001] The invention relates to a process for preparing triphenylchloromethane. Background technique [0002] At present, as an important pharmaceutical intermediate, triphenylchloromethane is more conducive to the nucleophilic substitution reaction because it is easy to form a stable form of trityl carbocation in the organic synthesis reaction, and can It acts as a space-occupying protection and is often used for group protection of drugs such as alcohols and amines, so it is widely used in the chemical and pharmaceutical fields. Triphenylchloromethane, also known as chlorotriphenylmethane, is a kind of off-white powder substance, easily soluble in benzene, toluene, petroleum ether, insoluble in water, but easily reacts to form triphenylmethanol after absorbing water. [0003] Due to problems such as low purity, low yield, and high pollution in the synthesis process of triphenyl chloride, researchers have continuously developed the synthesis process of trip...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/266C07C17/38C07C17/389C07C17/392C07C22/04
CPCC07C17/266C07C17/38C07C17/389C07C17/392C07C22/04
Inventor 沈文光潘文华叶新
Owner 江西华飞医药科技有限公司
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