A method for preparing 2,2-dichlorophenylacetonitrile

A technology of dichlorophenylacetonitrile and phenylacetonitrile, which is applied in the preparation of carboxylic acid nitriles, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high equipment requirements, unfavorable control, large energy consumption, etc., and achieve good safety , low equipment requirements and low energy consumption

Inactive Publication Date: 2018-12-18
南平铭正医药化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this reaction needs to feed two kinds of gases, HCl gas needs to be fed in the early stage, and chlorine gas needs to be fed in the later stage, and because HCl is continuously generated during the reaction process, the pressure will continue to increase. The continuous pressure relief and exhaust in the middle is very cumbersome, which is not conducive to the control of the reaction
Moreover, the pressurized reaction has high requirements on equipment, requires pressure-resistant sealing, high cost and high energy consumption

Method used

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  • A method for preparing 2,2-dichlorophenylacetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 1171g (10mol) phenylacetonitrile to the first reactor, heat to 110°C, and add another 1171g (10mol) benzylnitrile to the second reactor, also heat to 110°C, pass 1455g (20.5mol) of chlorine gas into the first reaction kettle, and continue heating under normal pressure at 110°C to react for 20 hours; the tail gas generated by the reaction is first passed into the second reaction kettle, and finally passed to the hydrochloric acid absorption tower. The liquid in the first reaction kettle was detected by GC, and the conversion rate of phenylacetonitrile was 99.4%. The liquid in the first reaction kettle was distilled under reduced pressure to obtain 1843 g of product 2,2-dichlorophenylacetonitrile, with a yield of 99.1%.

[0040] 2,2-Dichlorophenylacetonitrile NMR identification, the spectrum is as follows figure 1 Shown: 1 H NMR (400MHz, CDCl 3 ,δ,ppm):7.89-7.80(m,2H),7.55-7.45(m,3H).

Embodiment 2

[0042] Add 1171g (10mol) phenylacetonitrile to the first reaction kettle, heat to 100°C, and add another 1171g (10mol) benzylnitrile to the second reaction kettle, also heat to 100°C, pass chlorine gas 1475g (20.8mol) into the first reaction kettle, and continue to heat and react at normal pressure for 28 hours; the tail gas generated by the reaction is first passed into the second reaction kettle, and finally passed to the hydrochloric acid absorption tower. The liquid in the reaction kettle was detected by GC, and the conversion rate of phenylacetonitrile was 99.6%. The liquid in the first reaction kettle was distilled under reduced pressure to obtain 1850 g of the product 2,2-dichlorophenylacetonitrile, with a yield of 99.5%.

Embodiment 3

[0043] Embodiment 3: (cycle method)

[0044] The material in the second reactor in Example 2 (1171g (10mol) benzyl nitrile that has passed through last first reactor tail gas) is transferred in the first reactor, is heated to 100 ℃, simultaneously other 1171g (10mol) phenylacetonitrile is added to the second reaction kettle, also heated to 100°C, 1475g (20.8mol) of chlorine gas is passed into the first reaction kettle, and the heating reaction is continued at normal pressure for 28 hours; the tail gas generated by the reaction is first passed into the second reaction kettle In the kettle, it is finally passed to the hydrochloric acid absorption tower. The liquid in the reaction kettle was detected by GC, and the conversion rate of phenylacetonitrile was 99.8%. The liquid in the first reaction kettle was distilled under reduced pressure to obtain 1850 g of product 2,2-dichlorophenylacetonitrile, with a yield of 99.6%.

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Abstract

A method for preparing 2,2-dichlorophenylacetonitrile is disclosed. The method includes feeding chlorine into phenylacetonitrile under atmospheric pressure, heating and reacting the mixture, with theconversion ratio of the phenylacetonitrile being not less than 99.3%; and performing vacuum distillation to obtain the 2,2-dichlorophenylacetonitrile, with the yield of the 2,2-dichlorophenylacetonitrile being not less than 99.1%. The method is an extremely simple method for preparing the 2,2-dichlorophenylacetonitrile. The method is simple to operate, simple in device, safe and efficient and avoids adverse factors such as high requirements on pressurized chlorination devices, complex operation, low efficiency and poor safety performance.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a simple and convenient preparation method of 2,2-dichlorophenylacetonitrile. Background technique [0002] 2,2-dichlorophenylacetonitrile is a product in which two hydrogens on the methylene group in phenylacetonitrile are replaced by chlorine. It is an important raw material in chemical industry and can be used in the preparation of rubber additive ethyl dichlorophenylacetate. [0003] At present, many documents have reported the synthesis of 2,2-dichlorophenylacetonitrile, and different chlorination reagents can be used to carry out the α-position chlorination of benzylnitrile: such as 2,2-dichlorophenylacetonitrile can be synthesized from phenylacetonitrile and butyl The α-position hydrogen extraction is carried out in the base lithium reaction, and then obtained under the action of a chlorination reagent, and the yield is 87% (Synthesis, 2005, 7, 1136.), but butyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/35
CPCC07C253/30C07C255/35
Inventor 陈忠春冯清
Owner 南平铭正医药化学有限公司
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