Preparation method of n-2,6-diisopropylaniline perylene monoimide
A technology of diisopropylaniline and diisopropylphenyl, which is applied in the field of preparation technology of dyes, can solve the problems of high reaction temperature and pressure requirements, high production risk coefficient, complicated and complicated steps, etc., and achieves low reaction temperature, The effect of good safety and broad application prospects
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Embodiment 1
[0024] Mix and dissolve 1g (2.55mmol) of 3,4,9,10-perylenetetracarboxylic anhydride, 7.65mmol of zinc acetate, 3mL of water, and 17.85mmol of 2,6-diisopropylaniline in 10.2g of imidazole, Mix evenly, and react for 30 minutes in a microwave synthesizer with a set power of 80 watts at a temperature of 170°C to obtain a reaction solution; cool the reaction solution to room temperature, and add 400 mL of dichloromethane solution (V 二氯甲烷 :V 水 =1:1) dissolve, filter out the insoluble matter, separate the filtrate, take the organic phase and wash it twice with 300mL of 1.0mol / L hydrochloric acid solution, once with 300mL of water, and once with 300mL of saturated sodium chloride solution Wash once, pass the washed solution through a silica gel column, the eluent of the silica gel column is dichloromethane and petroleum ether with a volume ratio of 2:1, and separate to obtain N-2,6-diisopropylaniline perylene monoimide. The yield of the target compound was detected to be 64.1%.
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Embodiment 2
[0028] Mix and dissolve 1g (2.55mmol) of 3,4,9,10-perylenetetracarboxylic anhydride, 2.55mmol of zinc acetate, 2mL of water, and 20.4mmol of 2,6-diisopropylaniline in 5.1g of imidazole, Mix evenly, and react for 60 minutes in a microwave synthesizer with a set power of 80 watts at a temperature of 160°C to obtain a reaction solution; cool the reaction solution to room temperature, and add 400 mL of dichloromethane solution (V 二氯甲烷 :V 水 =1:1) dissolve, filter out the insoluble matter, separate the filtrate, take the organic phase and wash it twice with 300mL of 1.0mol / L hydrochloric acid solution, once with 300mL of water, and once with 300mL of saturated sodium chloride solution Wash once, pass the washed solution through a silica gel column, the eluent of the silica gel column is dichloromethane and petroleum ether with a volume ratio of 2:1, and separate to obtain N-2,6-diisopropylaniline perylene monoimide.
Embodiment 3
[0030] Mix and dissolve 1g (2.55 mmol) of 3,4,9,10-perylenetetracarboxylic anhydride, 10.2 mmol of zinc acetate, 4 mL of water, and 17.85 mmol of 2,6-diisopropylaniline in 10.2 g of imidazole, Mix evenly, and react for 20 minutes in a microwave synthesizer with a set power of 80 watts at a temperature of 180°C to obtain a reaction solution; cool the reaction solution to room temperature, and add 400 mL of dichloromethane solution (V 二氯甲烷 :V 水 =1:1) dissolve, filter out the insoluble matter, separate the filtrate, take the organic phase and wash it twice with 300mL of 1.0mol / L hydrochloric acid solution, once with 300mL of water, and once with 300mL of saturated sodium chloride solution Wash once, pass the washed solution through a silica gel column, the eluent of the silica gel column is dichloromethane and petroleum ether with a volume ratio of 2:1, and separate to obtain N-2,6-diisopropylaniline perylene monoimide.
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