Processes for producing 2,4,6-tris (hydroxyphenyl amino)-1,3,5-triazines and 2,4,6-tris (substituted phenylamino) -1,3,5, -triazines
a technology of hydroxyphenyl amino and triazines, which is applied in the field of processes, can solve the problems of difficult control of reaction activities of oh group and nh group, reaction needs a long time to go to completion, or hardly goes to completion, etc., and achieves the effect of short time and high yield
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[0036] The present invention will further be detailed referring to specific Examples. Materials, reagents, amount of use and ratio thereof, manipulation and so forth may appropriately be modified without departing from the spirit of the present invention. It is to be understood that the scope of the present invention is by no means limited to the specific examples described below.
example no.1
Example No. 1
Preparation of 2,4,6-tris(4′-hydroxyphenylamino)-1,3,5-triazine (III-a)
[0037]
[0038] In a 300 ml three-neck flask equipped with a stirrer, a thermometer and a dropping funnel, 3.68 g (0.02 mol) of cyanuric chloride was dissolved in 60 ml of methyl ethyl ketone. Subsequently, 6.55 g (0.06 mol) of p-aminophenol was added slowly to the solution at an inner temperature not higher than 5° C. After the addition, the solution was stirred for 30 minute, and 30 ml of an aqueous solution of 4.92 g (0.06 mol) sodium acetate was added dropwise to the solution with keeping an inner temperature of 10° C. After the dropwise addition, the solution was stirred for 30 minutes at room temperature and was reacted with refluxing for 3 hours. During the reaction, the mixed solvent of methyl ethyl ketone and water was separated into two phases. When the reaction was complete, the reaction solution was poured into 500 ml of ice water to be crystallized. After the filtration, the obtained cryst...
example no.2
Example No. 2
Preparation of Compound E-31
[0041]
[0042] In a 300 ml three-neck flask equipped with a stirrer, a thermometer and a dropping funnel, 32.3 g (0.08 mol) of 2,4,6-tris(4′-hydroxy phenylamino)-1,3,5-triazine (III-a), prepared in Example No. 1, and 0.4 g of dimethylamino pyridine were dissolved in 200 ml of dimethylacetamide. Subsequently, 43.4 g (0.288 mol) of Compound (V-a) was added dropwise to the solution at an inner temperature of not higher than 10° C. After that, 50 ml (0.36 mol) of triethylamine was added dropwise to the solution with keeping an inner temperature of 20° C. After the dropwise addition, the solution was reacted for 5 hours while an inner temperature was kept at room temperature. When the reaction was complete, the reaction solution was poured into 300 ml of water and the organic layer was extracted with 500 ml of ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and evaporated of ethyl acetate under reduced pressure....
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