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Preparation method for hydrazobenzene compounds

A technology for hydrogenated azobenzene and compounds, applied in chemical instruments and methods, hydrazine preparation, chemical/physical processes, etc., can solve the problems of high consumption, unfriendly environment, complicated preparation process, etc., achieve high yield, avoid a large number of effect used

Active Publication Date: 2017-03-15
FUZHOU UNIV
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  • Application Information

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Problems solved by technology

Solve the problems of complex preparation process of hydroazobenzene compounds, large consumption and unfriendly environment

Method used

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  • Preparation method for hydrazobenzene compounds
  • Preparation method for hydrazobenzene compounds
  • Preparation method for hydrazobenzene compounds

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preparation example Construction

[0021] Preparation of gold / boron nitride composite catalyst: hexagonal boron nitride colloid was prepared according to the preparation method of hexagonal boron nitride in CN201510022305.7 patent. Add 2 mL, 10 g / L chloroauric acid and 2 mL, 31 mg / mL lysine solution to 5 mL, 20.1 mg / mL hexagonal boron nitride colloid, stir vigorously for 30 min, then add 10 mL dropwise to the solution , 3.8 mg / mL sodium borohydride, added dropwise within 20 min, continued to stir for an hour, kept in the dark for 16 h, filtered and washed with water and absolute ethanol, dried, and the gold / boron nitride nanosheet composite structure catalyst was obtained . Catalysts with different gold contents were marked as 3.7% gold / boron nitride, 8.2% gold / boron nitride, 14.7% gold / boron nitride, 20.9% gold / boron nitride, 30.1% gold / boron nitride according to mass ratio boron.

[0022] The present invention uses nitrobenzene compound as the main raw material, adopts 20.9% gold / boron nitride compound as c...

Embodiment 1

[0027] Add 0.31 mmol of nitrobenzene, 0.06 mmol of potassium hydroxide, 3 mL of isopropanol and 10 mg of gold / boron nitride catalyst into the reaction tube to maintain a nitrogen atmosphere; immerse the mixed reaction system in 90 o In an oil bath of C, react for 0.5 hours; filter the reaction solution while hot, and analyze it with a UV-visible spectrophotometer to obtain a yield of 99% of hydroazobenzene.

Embodiment 2

[0029] 0.31 mmol of nitrobenzene, 0.06 mmol of potassium hydroxide, 3 mL of isopropanol and 10 mg of 20.9% gold / boron nitride catalyst were added to the reaction tube in an air atmosphere; the mixed reaction system was immersed in 90 o In the oil bath of C, react for 1 hour; filter the reaction solution while it is hot, and analyze it with an ultraviolet-visible spectrophotometer, and the yield of hydroazobenzene is more than 90%.

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Abstract

The invention discloses a preparation method for hydrazobenzene compounds, belonging to the technical field of fine chemical engineering products. The preparation method improves the current situation that hydrazobenzene compounds are heard to prepare and overcomes the problems of severe preparation conditions, high pollution and the like. According to the preparation method, nitrobenzene compounds are used as raw materials; a gold / boron nitride nanosheet compound is used as a catalyst; potassium hydroxide maintains a slightly alkaline environment; and the hydrazobenzene compounds are prepared through one-step reduction in a normal-pressure air or nitrogen atmosphere. High-efficiency preparation of the hydrazobenzene compounds is realized without any special atmosphere and additional pressure. The preparation method is simple, low in environmental pollution and beneficial for large-scale industrial production, and has substantial economic and social benefits.

Description

technical field [0001] The invention discloses a method for preparing hydroazobenzene compounds and relates to the technical field of fine chemical products. Background technique [0002] Hydroazobenzene compounds can be widely used in medicines, pesticides, dyes and other fields, and are important intermediates in organic synthesis. The current industrial production method is mainly the catalytic hydrogenation method, by adding a large amount of alkali and metal, and passing in hydrogen gas, the nitrobenzene compounds are reduced to hydroazobenzene compounds. However, the alkali and metals in the reaction process are also consumed in a large amount, which is difficult to recycle, which seriously affects the cost of preparation, and there are too many by-products, and the reaction under high pressure has certain dangers. [0003] Therefore, the preparation of hydroazobenzene compounds by highly selective and low-consumption catalytic methods has attracted extensive attentio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/22B01J27/24
CPCB01J27/24C07C241/02C07C243/22
Inventor 黄彩进刘秋文
Owner FUZHOU UNIV
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