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Method for preparing 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl) aniline

A technology of methyl aniline and methyl, which is applied in the field of preparation of perfluoroalkylaniline derivatives, and can solve problems such as safety and insecurity

Active Publication Date: 2012-10-17
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Reaction at higher pressure significantly increases equipment requirements and brings unsafe factors in terms of safety

Method used

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  • Method for preparing 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl) aniline
  • Method for preparing 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl) aniline

Examples

Experimental program
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Effect test

Embodiment 1

[0052]Add the liquid mixture of 20ml water and 20ml tert-butyl methyl ether in 1 liter closed reactor, then add 1 gram (9.3mmol) 2-methylaniline, 2.3 gram (12.5 mmol) sodium dithionite, 1.1 gram (13 mmol) Sodium bicarbonate and 0.4 gram (1.2 mmol) tetrabutylammonium bisulfate, start stirring, open the frozen brine of condenser, make the internal temperature of condenser be controlled at-20 ℃, control reactor internal temperature at 20-30 ℃, Continuously and slowly add 3.1 grams (12.5 mmol) of 1,1,1,2,3,3,3-heptafluoro-2-bromopropane with a micro-feed pump, vent the tail gas of the condenser into the tail gas treatment system, and the resulting mixture Stir at room temperature for 2 hours. Separate the organic layer, extract the aqueous layer with 20ml ethyl acetate, combine the extract with the organic layer, and wash with 2N aqueous hydrochloric acid, 5% sodium carbonate and saturated sodium chloride solution successively, and wash the organic layer with anhydrous magnesium s...

Embodiment 2

[0055] Open the manhole cover of 1000 liters of glass reaction, add the mixture of 200 liters of water and 200 liters of methyl tert-butyl ether in the reactor, then add 27.5 kg of 2-methylaniline, 40 kg of sodium dithionite, 24 kg of sodium bicarbonate and 4 kg of tetrabutylammonium bisulfate, turn on the motor to stir after adding, and after mixing evenly, turn on the frozen brine of the condenser to control the internal temperature of the condenser at -20°C, and the exhaust gas of the condenser Vent to the tail gas treatment system, control the internal temperature of the reactor between 20-30 ℃, start to continuously inject 67 kg of 1,1,1,2,3,3,3-heptafluoro-2 with a metering pump -bromopropane, the system pressure in the reactor is below 0.5 bar during the reaction, and the rear system pressure is normal pressure, and the time for pumping 1,1,1,2,3,3,3-heptafluoro-2-bromopropane is 0.5-4 hours, after feeding, keep warm for 4 hours. The reactants were separated into layer...

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Abstract

The invention relates to a method for preparing 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl) aniline which is obtained by reaction of 2-methylaniline with heptafluoro-2-bromopropane under the effect of an initiator. According to the method, the raw materials are low in cost, the reaction condition is mild, and the process is simple and accessible, so that the method is an ideal industrialized production method.

Description

technical field [0001] The invention relates to a preparation method of perfluoroalkylaniline derivatives, in particular to a 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl ) Preparation method of aniline. Background technique [0002] Perfluoroalkylaniline derivatives are a class of fluorine-containing fine chemicals with broad application prospects, and can be widely used as raw materials or intermediates for medicine, pesticides, surfactants, coatings, rubber, etc. Therefore, it is necessary to develop a safe, Low-cost industrial production methods have very important economic value. [0003] The known methods of perfluoroalkylaniline derivatives with industrial production value are mainly developed by Nippon Norochemical Co., Ltd., and corresponding patents have been applied for. The patent numbers are: CN1257861A and JP2003335735A. In addition, Germany Saito Co., Ltd. also applied for the process technology of the reaction under pressure, and its patent number is CN10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/74
Inventor 虞小华姚汉清孔小林向绍基郑韵红鲍樟水
Owner SINOCHEM LANTIAN
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