Catalysis synthesis method for nitrobenzene ether catalysis synthesis method for paranitroanisole

A technology of p-nitroanisole and p-nitrophenol, which is applied in the field of catalytic synthesis of p-nitroanisole, can solve the problems of high cost and troublesome synthesis, and achieve the effect of simple separation

Inactive Publication Date: 2008-12-03
JIANGSU POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the polymer phase transfer catalyst is a catalyst with good effect and can be reused, its synthesis is troublesome and the cost is also high. The alkali used in the synthesis process is sodium hydroxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The activated carbon impregnated with 20% potassium hydroxide is used as a catalyst, the amount of catalyst is 5% of the raw material quality, the molar ratio of raw materials p-nitrophenol: dimethyl carbonate is 1: 10, the reaction temperature is 150 ° C, and the reaction time is 4 hours , the p-nitrophenol conversion rate is 98.8%, and the p-nitroanisole selectivity is 100%.

Embodiment 2

[0017] The activated carbon impregnated with 5% potassium hydroxide is used as a catalyst, the amount of catalyst is 5% of the raw material quality, the molar ratio of raw materials p-nitrophenol: dimethyl carbonate is 1: 10, the reaction temperature is 150 ° C, and the reaction time is 4 hours , the conversion rate of p-nitrophenol was 7.1%, and the selectivity of p-nitroanisole was 100%.

Embodiment 3

[0019] The active carbon impregnated with 30% potassium hydroxide place is as catalyst, and catalyst consumption is 5% of raw material quality, and raw material molar ratio p-nitrophenol: dimethyl carbonate is 1: 10, and reaction temperature is 150 ℃, and reaction time is 4 hour, p-nitrophenol conversion rate is 83.2%, and p-nitroanisole selectivity is 96.4%.

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Abstract

The invention relates to a method for synthesizing paranitroanisole. The raw materials used by the method are green chemicals dimethyl carbonate (DMC) and p-nitrophenol, and the catalyst is NaY molecular sieve, activated aluminum oxide or activated carbon which is impregnated by alkali metals or alkaline-earth metal compounds. Good conversion rate of the raw materials and good selectivity of target products can be obtained by using the method provided by the invention under the reaction conditions that: the temperature is between 90 and 200 DEG C, and the reaction time is between 1 and 5 hours; the mol ratio of the p-nitrophenol to the dimethyl carbonate of the raw materials is between 1 to 5 and 1 to 15, and the amount of the catalyst is 2 to 20 percent of the mass of the raw materials, wherein, the conversion rate of the p-nitrophenol can reach over 64 percent, and the selectivity of the paranitroanisole can reach 100 percent. The method takes the DMC as a methylated reagent to actually realize a green synthetic route, takes solid alkali as the catalyst, and is superior to the prior synthetic method of homogeneous catalysis or phase-transfer catalysis; and the catalyst is simple to separate and can be reused.

Description

technical field [0001] The invention relates to the field of organic chemical industry, in particular to a method for catalytically synthesizing p-nitroanisole. Background technique [0002] p-nitroanisole, also known as p-nitroanisole, colorless or light yellow prismatic crystals, density 1.2540g / cm 3 , melting point 54°C, boiling point 274°C, easily soluble in alcohol, ether and hot petroleum ether, slightly soluble in cold petroleum ether, insoluble in water, can be used as a dye intermediate and other organic synthesis raw materials, and can also be used as a base for medicine and pesticides It can also be used as an inert solvent in organic synthesis. [0003] At present, the method of domestic production of p-nitroanisole mostly adopts the synthetic route of alkoxylation, that is, using p-nitrochlorobenzene, methanol and sodium hydroxide as raw materials, and performing methoxylation reaction under a pressure of 0.3MPa , and then distilled under reduced pressure to o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/38C07C201/12
Inventor 李永昕薛冰蔡明明
Owner JIANGSU POLYTECHNIC UNIVERSITY
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