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Green synthesizing method of triphenylchloromethane

A technique for the synthesis of triphenylchloromethane, which is applied in chemical instruments and methods, organic chemistry, preparation of halogenated hydrocarbons, etc., can solve problems such as unfavorable large-scale production, difficulties in use and transportation, and difficult control, and achieve production costs Low, less waste, environment-friendly effect

Active Publication Date: 2010-06-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using acetyl chloride, due to its active nature, it is easy to cause difficulties in use and transportation
The use of hydrogen chloride gas has high requirements on production equipment, and it is not easy to control, which is not conducive to large-scale industrial production. Therefore, it is imperative to find a green and effective chlorination reagent.

Method used

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  • Green synthesizing method of triphenylchloromethane
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 1000ml four-necked flask equipped with a thermometer and mechanical stirring, add 130g (0.5mol) of triphenylmethanol and 50g of bis(trichloromethyl)carbonate, dissolve and stir with 200ml of toluene, and then add 1.5 g of triethylamine. g, heated to 80°C. The reaction temperature was maintained and stirred for 2 hours. After the reaction was completed, toluene was recovered by distillation under reduced pressure, and the crude product was recrystallized from petroleum ether to obtain 136.5 g of white pure product with a yield of 98% and a melting point of 109-111°C.

Embodiment 2

[0020] In a 1000ml four-neck flask equipped with a thermometer and mechanical stirring, add 130g (0.5mol) of triphenylmethanol and 80g of bis(trichloromethyl)carbonate, dissolve and stir with 200ml of dichloromethane, and then add 1.5 mol of pyridine. g, heated to 40°C. The reaction temperature was maintained and stirred for 5 hours. After the reaction was completed, dichloromethane was recovered by distillation under reduced pressure, and the crude product was recrystallized from petroleum ether to obtain 124 g of white pure product with a yield of 89% and a melting point of 109-112°C.

Embodiment 3

[0022] In a 1000ml four-necked flask equipped with a thermometer and a mechanical stirrer, add 130g (0.5mol) of triphenylmethanol and 80g of bis(trichloromethyl) carbonate, and use 200ml of toluene / chlorobenzene (V / V=1: 1) The mixed solvent is dissolved and stirred, and heated to 80°C. The reaction temperature was maintained and stirred for 2 hours. After the reaction was completed, the solvent was recovered by distillation under reduced pressure, and the crude product was recrystallized from petroleum ether to obtain 129 g of pure product with a yield of 93% and a melting point of 109-112°C.

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Abstract

The invention discloses a green synthesizing method of triphenylchloromethane. The synthesizing method comprises the following steps of: using triphenylmethanol as raw material; reacting the triphenylmethanol with triphosgene in an organic solvent for 0.1-20 hours at a temperature of -20-150 DEG C; after reacting, separating to obtain a crude product; and recrystallizing the crude product to obtain the triphenylchloromethane, wherein the mass ratio of the triphenylchloromethane to the triphosgene is 1:(0.33-2). The synthesizing method has the advantages of reasonable process, high reaction yield, low production cost, less three waste and simple aftertreatment.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing a pharmaceutical intermediate triphenylchloromethane. (2) Background technology [0002] Triphenylchloromethane is an important pharmaceutical intermediate and chemical raw material. Due to its unique structure and properties different from ordinary organic chlorides, it is widely used in the protection of hydroxyl groups in organic and pharmaceutical synthesis. [0003] Before the present invention is presented, the chemical synthesis method of triphenylchloromethane in the prior art is mainly prepared by triphenylmethanol and thionyl chloride, acetyl chloride or hydrogen chloride gas chlorination. Such as literature [J.Am.Chem.Soc., (1989), 111(11), 3966-72.] using thionyl chloride as substrate reaction to obtain the target product. The literature [Organic Syntheses, 23, 1943.] used acetyl chloride as chloride to prepare triphenylchloromethane. As a traditional production process, the thionyl c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C22/04C07C17/16
Inventor 苏为科金灿陈俊
Owner ZHEJIANG UNIV OF TECH
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