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Recycling and reuse technology for preparing triphenylchloromethane

A technology of triphenylchloromethane and cyclic application, which is applied in the preparation of halogenated hydrocarbons, the production of bulk chemicals, organic chemistry, etc., can solve the problem that the purity of recycled materials cannot be well guaranteed, tar-like substances are easily generated, and the production site is affected. environment and other issues, to achieve the effect of convenient source of raw materials, controllable impurities and low price

Inactive Publication Date: 2019-09-06
LINHAI HUANAN CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. A large amount of sulfur dioxide and hydrogen chloride waste gas is generated during the production process, and tail gas absorption is required. A large amount of gas has high requirements for tail gas absorption. Generally, multi-stage series absorption is required. If the reaction speed is too fast, acid gas overflow will affect the production site environment and equipment ;
[0011] 2. The reaction of thionyl chloride requires proper heating, or a large excess of thionyl chloride, which brings a certain pressure to the post-treatment;
[0012] 3. There are many side reactions, low yield, easy to produce tar-like substances, and post-processing is very troublesome. Since the purity of recycled materials cannot be well guaranteed, the product purity is not ideal, and crystallization and purification are required.
These factors all restrict large-scale recycling

Method used

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  • Recycling and reuse technology for preparing triphenylchloromethane
  • Recycling and reuse technology for preparing triphenylchloromethane
  • Recycling and reuse technology for preparing triphenylchloromethane

Examples

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example 1

[0045] Synthesis of Triphenylchloromethane

[0046] Recover 500mL of triphenylmethanol toluene solution (containing 50g of triphenylmethanol with a purity of 98% or more), add 50mL of concentrated hydrochloric acid, stir at 25°C for 5h, stand for 0.5h to separate the water layer, control the vacuum and concentration temperature figure 2 , Attached with standard product figure 1 Consistent.

example 2

[0048] Synthesis of Triphenylchloromethane

[0049] Recover 500mL of triphenylmethanol toluene solution (containing 50g of triphenylmethanol, with a purity of 98% or more), add 50mL of concentrated hydrochloric acid, 5g of calcium chloride, stir for 5h at 25°C, stand for 0.5h to separate the water layer, control the vacuum and Concentrate temperature <30℃, concentrate toluene to dryness to obtain a solid containing triphenylchloromethane, raise the temperature to 60℃, continue drying for 5h, weigh 51.4g of triphenylchloromethane, yield: 96.0%, content : 99.3%.

example 3

[0051] Synthesis of Triphenylchloromethane

[0052] Recover 500mL of triphenylmethanol methyl isobutyl ketone solution (containing 50g of triphenylmethanol, purity above 98%), add 50mL of hydrochloric acid, 5g of calcium chloride, stir at 25°C for 5h, stand for 0.5h to separate the water layer, Control the degree of vacuum and the concentration temperature <30℃, concentrate the methyl isobutyl ketone to dryness to obtain a solid containing triphenylchloromethane, raise the temperature to 60℃, continue drying for 6h, weigh to obtain triphenylchloromethane 51.4 g, yield: 96.0%, content: 99.0%.

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Abstract

The invention provides a recycling and reuse technology for preparing triphenylchloromethane. The technology comprises the following steps that hydrochloric acid or a mixture of the hydrochloric acidand Lewis acid is added into a solvent of triphenylcarbinol, stirring is conducted at a certain temperature, after a reaction is finished, separation is conducted, or after separation, recrystallization is further conducted, and the triphenylchloromethane is obtained after drying, wherein the reaction equation is shown in the description. The reuse technology is a recycling and reuse technology which is wide in raw material source, low in price and simple in production process operation and causes little pollution, and the technology is very suitable for commercialized production.

Description

Technical field [0001] The invention relates to a process for preparing triphenylmethyl chloride in a cycle, more specifically to a process for preparing triphenylchloromethane in a process of producing antihypertensive sartan drug intermediates [0002] technical background [0003] Triphenylchloromethane, white crystal, insoluble in water, easily soluble in benzene, carbon disulfide, petroleum ether, n-hexane, slightly soluble in alcohol and ether, and becomes triphenylmethanol after absorbing water. Triphenylchloromethane is one of the basic organic raw materials commonly used in the field of medicine and chemical industry. In the process of organic chemical industry and drug synthesis, triphenylmethyl and its similar protecting groups are easy to up and down, and have mild conditions and high stability. With the characteristics of large steric hindrance, it has developed into one of the most commonly used amino or hydroxyl protecting groups, especially in the selective protecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C22/04C07D257/04
CPCC07C17/16C07D257/04C07C22/04C07C257/04
Inventor 张露涂国良许建跃郭欣靳和平王甦胡奇杨森刘恒
Owner LINHAI HUANAN CHEM CO LTD
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