Fluorane color former and preparation method thereof
A technology of couplers and fluoranes, applied in the field of fluorane couplers and their preparation, can solve the problems of poor weather resistance and compatibility, low color sensitivity of couplers, and high production cost, and achieves low price and high product purity. , the effect of easy operation
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Embodiment 1
[0032] Synthesis of 3-(N-ethyl-N-isopentyl)amino-6-methyl-7-(N-carboxanilide)ylfluoran
[0033] Weigh 108g of 98% sulfuric acid and put it into the reaction bottle, cool it in an ice-water bath (control the temperature at 5-8°C), and slowly add the raw material 2-hydroxyl-4-(N-ethyl-N-isoamyl) under stirring condition Amino-2-carboxy-benzophenone 14.6g, add in about 4 hours; slowly add N-formyl-2-methyl-4-methoxydiphenylamine 9.4g, add in about 4 hours; keep warm at 5°C for 20 hours; Under the condition of stirring, the reaction liquid was slowly poured into 200 g of ice water, and a large amount of solid was precipitated, filtered and washed to obtain 86 g of pink filter cake.
[0034] Measure 110ml of toluene, 50ml of water, and 30ml of 30% sodium hydroxide aqueous solution into the reaction flask, slowly add the above filter cake into the reaction flask under stirring conditions, slowly raise the temperature to reflux for 2 hours, separate liquid, and 100ml of hot water Wa...
Embodiment 2
[0036] Synthesis of 3-(N-ethyl-N-isopentyl)amino-6-methyl-7-(N-carboxanilide)ylfluoran
[0037] Weigh 108g of 105% oleum and put it into a reaction flask, cool in an ice-water bath (temperature control at 5-8°C), and slowly add the raw material 2-hydroxy-4-(N-ethyl-N-isoamyl Base) amino-2-carboxy-benzophenone 14.6g, add in about 4h; slowly add N-formyl-2-methyl-4-methoxydiphenylamine 7.9g, add in about 4h; keep warm at 10°C 20h; under the condition of stirring, the reaction solution was slowly poured into 200g of ice water, a large amount of solid was precipitated, filtered and washed to obtain 92g of pink filter cake.
[0038] Measure 110ml of chlorobenzene, 60ml of water, and 30ml of 30% sodium hydroxide aqueous solution into the reaction flask, slowly add the above filter cake into the reaction flask under stirring conditions, slowly raise the temperature to reflux for 2 hours, separate liquid, and heat 100ml Wash the organic phase with water, decolorize with 0.5g activate...
Embodiment 3
[0040] Synthesis of 3-dibutylamino-6-methyl-7-(N-carboxanilide) fluoran
[0041] Weigh 136g of 98% sulfuric acid and put it into the reaction flask, cool in an ice-water bath (temperature control at 5-8°C), and slowly add the raw material 2-hydroxy-4-dibutylamino-2-carboxy-benzophenone 23.4 g, added in about 4 hours; slowly added 14.6 g of N-formyl-2-methyl-4-methoxydiphenylamine, added in about 4 hours; kept at 0°C for 20 hours; under stirring conditions, slowly poured the reaction solution into In 400 g of ice water, a large amount of solids were precipitated, filtered and washed to obtain 118 g of pink filter cake.
[0042] Measure 180ml of toluene, 75ml of water, 52ml of 30% sodium hydroxide aqueous solution into the reaction flask, slowly add the above filter cake into the reaction flask under stirring conditions, slowly raise the temperature to reflux reaction for 2h, separate liquid, 150ml of hot water Wash the organic phase, decolorize with 1g activated carbon, heat f...
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