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A kind of synthetic method of diphenylmethylamine

A synthesis method and technology of diphenylmethylamine, applied in the field of synthesis of diphenylmethylamine, can solve the problems of easy explosion and high cost, and achieve the effect of high yield

Active Publication Date: 2017-04-12
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the amount of indium used is twice that of the substrate, the cost is high, and there is a risk of explosion

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  • A kind of synthetic method of diphenylmethylamine

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[0016] Implement the synthetic method of a kind of diphenylmethylamine provided above of the present invention. It uses benzophenone as the starting material, reacts with hydroxylamine hydrochloride to generate benzophenone oxime, and further obtains benzhydrylamine under the action of Bacillus cereus. The reaction equation and synthesis steps are as follows:

[0017]

[0018] (1) Synthesis of benzophenone oxime

[0019] The reaction raw materials are benzophenone, hydroxylamine hydrochloride, 95% ethanol, and sodium hydroxide, and the ratio thereof is W:W:V:W=1.67:1:3.33:1.83. Add benzophenone, hydroxylamine hydrochloride, and ethanol to the reaction flask in sequence, and gradually add sodium hydroxide while stirring at room temperature. After the addition was completed, the temperature was raised to 88° C. for 2 hours. After cooling down, the reaction solution was poured into dilute hydrochloric acid solution to precipitate a white solid, which was filtered to obtain ...

Embodiment 1

[0026] Implement a kind of synthetic method of diphenylmethylamine, and its described method is to carry out according to the following steps:

[0027] 1) Synthesis of benzophenone oxime

[0028] Put 10 g of benzophenone, 6 g of hydroxylamine hydrochloride, and 20 mL of 95% ethanol into the reaction flask, stir and dissolve, and then add 11 g of solid sodium hydroxide in portions. After the addition, the reaction solution was heated to 88°C for 2 hours, and then poured into dilute hydrochloric acid solution, a white solid appeared, which was filtered to obtain 10.7 g of benzophenone oxime, with a yield of 99%.

[0029] 2) Synthesis of diphenylmethylamine

[0030] Put 0.25g of benzophenone oxime and 5mL of 95% ethanol into the reaction bottle, and add the concentration of 5×10 after the solution becomes clear. 7 CFU / mL Bacillus cereus solution 50mL, shake the reaction in a shaker at a constant temperature of 30°C (rotating speed 200r / min). When TLC detects that there is no r...

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Abstract

The invention discloses a synthesis method for benzhydrylamine. The synthesis method comprises the following steps: adopting benzophenone and oxammonium hydrochloride as raw materials for reaction to obtain benzophenone oxime; reducing the benzophenone oxime into the benzhydrylamine under the action of ceraceous bacillus. The novel synthesis method that the method is mild in reaction conditions, simple to operate, high in reaction yield, free from contamination, and low in cost.

Description

technical field [0001] The present invention relates to a synthesis method of diphenylmethylamine, especially a kind of synthesis method of benzophenone oxime with benzophenone as raw material, and then reducing benzophenone oxime with Bacillus cereus to generate diphenylmethylamine resolve resolution. Background technique [0002] Diphenylmethylamine is a fine chemical intermediate. Tetrahedron 2005, 61:11686-11691 reported that benzophenone imine was reduced to diphenylmethylamine under light with a yield of 80%. Tetrahedron Letters, 2010,51: -55210212 reported that under microwave assistance, benzophenone, ammonium acetate, sodium borocyanide (NaCNBH 3 ) reacted to generate diphenylmethylamine with a yield of 85%. The disadvantage of this method is that sodium borocyanide is more expensive. Bull. Korean Chem. Soc., 2011,32(9):3448-3452 reported NaBH 4 / ZrCl 4 / Al 2 o 3 The reduction of benzophenone oxime to benzhydrylamine has a yield of 98%. The disadvantage of t...

Claims

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Application Information

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IPC IPC(8): C12P13/00C12R1/085
Inventor 邢俊德魏文珑张照昱孙彦云
Owner TAIYUAN UNIV OF TECH