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ChemicalBook CAS DataBase List 1,2-Dihydro-2,2,4-trimethylquinoline
147-47-7

1,2-Dihydro-2,2,4-trimethylquinoline synthesis

14synthesis methods
-

Yield:147-47-7 99.6%

Reaction Conditions:

with titanium isopropoxide at 120; for 5 h;Catalytic behavior;Reagent/catalyst;Temperature;

Steps:

2 Example 2

Continuous tower reaction mode: The weight ratio of the feed of tetraisopropyl titanate, aniline and acetone is controlled to be 1:450:1100.The aniline is continuously fed from the top of the tower. After acetone is vaporized, it is fed from the bottom of the tower and continuously reacted in the tower. The reaction pressure is normal pressure.The reaction temperature is 120 °C and the residence time of the material in the column is 5 hours. Excess acetone and water produced by the reaction pass through the fractionation tower connected to the top of the reaction tower.At the same time, acetone was recovered and the water produced by the separation reaction was reacted. The polycondensation solution of the anti-aging agent TMQ continuously flowed into the receiving tank at the bottom of the reactor. The conversion of aniline was 80.4%.After the antioxidant TMQ polycondensation solution, plus 5% sodium hydroxide 3g, neutralized to weakly alkaline, static stratification, the upper oil phase after -0. 098MPa vacuum, vacuum distillation recovery of unreacted aniline, not The TMQ monomer was polymerized to control the material temperature at 230°C (the recovered aniline and monomer were continuously used in the reaction), and the kettle solution was granulated to obtain the antioxidant TMQ finished product. The yield of the continuous process was 83.2%.Among them, the content of antioxidant TMQ effective body 74.2%; aniline and monomer sets for the reaction, the product TMQ effective yield of 99.6%.

References:

CN108003095,2018,A Location in patent:Paragraph 0021-0025

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