Construction and application of 2,6-dibromopyridine oxidation system
A technology of dibromopyridine and oxidation system, applied in the direction of organic chemistry and the like, can solve the problems of serious environmental pollution, expensive reagents, and a large amount of waste water, and achieves the effects of good catalytic activity, reduced synthesis cost, and reduced corrosion.
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[0033] The preparation method of each ionic liquid used in the present invention can operate with reference to the preparation method of catalyst in "Chemical Engineering Journal" 2011,172, specifically as follows:
[0034] One, the preparation of N,N-dimethylbenzylaminopropanesulfonic acid trifluoroacetic acid ionic liquid is:
[0035] Weigh 12.2g (0.1mol) of 1,3-propane sultone into a 100mL reaction flask, then add 50mL of ethyl acetate, stir evenly, cool the reaction system to 0°C, and drop 13.5 g (0.1mol) N,N-dimethylbenzylamine, continue to stir for 30 minutes after the dropwise addition, then raise the temperature to 60°C, and stir at constant temperature for 2 hours. Finish the reaction, suction filter, wash the filter cake, and dry to obtain white solid N,N-dimethylbenzylaminopropanesulfonate. Take 25.8g (0.1mol) N,N-dimethylbenzylaminopropanesulfonate and dissolve it in 60mL deionized water, N 2 Slowly add 11.4 g (0.1 mol) of trifluoroacetic acid dropwise to the sol...
Embodiment 1
[0039]Add 3g (0.0125mol) 2,6 dibromopyridine, 25g N,N-dimethylbenzylaminotrifluoroacetic acid ionic liquid, 5.7g 30% (0.05mol) hydrogen peroxide, 0.15 g cerium trifluoromethanesulfonate, reacted at 90°C for 4h, cooled to room temperature; added chloroform to the reaction system for extraction (20mL×3 times), combined the organic phases, and used 5% NaHCO 3 Solution (about 10 mL) washed the organic phase with water, and the organic phase was distilled to remove chloroform to obtain an off-white solid, recrystallized from methanol, and the white needle-like crystals obtained were N-dibromopyridine oxide (that is, N-oxide-2,6- Dibromopyridine), the yield is 83.6%. The water layer (ionic liquid aqueous solution) was dewatered under reduced pressure to obtain the ionic liquid, which was dried in vacuum (i.e., 75°C (1×10 -4 Pa) Vacuum dried overnight) and then applied.
Embodiment 2-9
[0041] The cerium trifluoromethanesulfonate in Example 1 was changed to the metal trifluoromethanesulfonate salt as described in Table 1 below, and the dosage remained unchanged, and the rest were the same as in Example 1.
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