Azo-compound
An azo compound, methyl technology, applied in the direction of azo dyes, monoazo dyes, organic chemistry, etc., can solve problems such as poor performance of environmental protection pressure disperse dyes
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Embodiment 1
[0086] Embodiment 1 naphthalene ring compound 2-1 (R 1 for hydrogen, R 2 For the preparation of methyl)
[0087]
[0088] At room temperature, in a dry 100ml three-necked flask, add 21.7g methyl chloroacetate (compound 5, R 2 methyl), and then add 19.09g of 1-naphthylamine, 8.5g of anhydrous sodium carbonate and 3.46g of sodium bromide while stirring, stir evenly, and then slowly raise the temperature to 100°C for reaction. The reaction was monitored by HPLC until the reaction of 1-naphthylamine was complete. Add about 70ml of water to dissolve the solid, slowly raise the temperature to 70°C and separate the layers while hot, collect the organic phase, add 50ml of water, adjust the pH to neutral with 30% aqueous sodium hydroxide solution at room temperature, then slowly raise the temperature to 70°C, and Heat layering, collect organic phase, decompression distillation removes moisture, obtains naphthalene ring compound 2-1 (R 1 for hydrogen, R 2 is methyl) 27.35g, yiel...
Embodiment 2
[0089] Embodiment 2 naphthalene ring compound 2-4 (R 1 is methyl, R 2 for the preparation of ethyl)
[0090]
[0091] At room temperature, in a dry 100ml three-necked flask, add 24.51g ethyl chloroacetate (compound 5, R 2 ethyl), and then add 24.19g of N-methyl 1-naphthylamine, 8.5g of anhydrous sodium carbonate and 3.46g of sodium bromide while stirring, stir evenly, and then slowly raise the temperature to 120°C and keep it warm for reaction. The reaction was monitored by HPLC until the reaction of N-methyl-1-naphthylamine was complete. Add about 70ml of water to dissolve the solid, slowly raise the temperature to 70°C and separate the layers while hot, collect the organic phase, add 50ml of water, adjust the pH to neutral with 30% aqueous sodium hydroxide solution at room temperature, then slowly raise the temperature to 65°C, Heat layering, collect organic phase, decompression distillation removes moisture, obtains naphthalene ring compound 2-4 (R 1 is methyl, R 2 ...
Embodiment 3
[0092] Embodiment 3 naphthalene ring compound 2-6 (R 1 is ethyl, R 2 for the preparation of ethyl)
[0093]
[0094] At room temperature, in a dry 100ml four-necked flask, add 30ml absolute ethanol, 21.26g ethyl chloroacetate (compound 5, R 2 ethyl), then add 22.83g of N-ethyl 1-naphthylamine, 8.5g of anhydrous sodium carbonate and 3.46g of sodium bromide while stirring, stir evenly, and then slowly heat up to 100°C for reaction under reflux. The reaction was monitored by HPLC until the reaction of N-ethyl-1-naphthylamine was complete. Cool down to room temperature, and distill off ethanol and excess ethyl chloroacetate under reduced pressure. Add about 70ml of water to dissolve the solid, slowly raise the temperature to 70°C and separate the layers while hot, collect the organic phase, add 50ml of water, adjust the pH to neutral with 30% aqueous sodium hydroxide solution at room temperature, then slowly raise the temperature to 70°C, and Heat layering, collect organic ...
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