A kind of synthetic method of medicine intermediate triazole compound
A synthesis method and compound technology, which is applied in the field of organic synthesis, synthesis of triazole compounds, and synthesis of heteroatom-containing compounds, can solve the problems that cannot meet the needs of synthesis or preparation of pharmaceutical compounds, and achieve good application prospects and industrialization potential , high yield, broad marketing prospects
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Embodiment 1
[0038]
[0039] At room temperature, add 100mmol of the above formula (I) compound, 120mmol of the above formula (II) compound, 100mmol of the above formula (III) compound, 1mmol [Pd(CH 3 EN) 4 ](BF 4 ) 2 , 10 mmol 1-ethyl-3-methylimidazolium dicyanamide salt and 300 mmol DAB CO, the temperature was raised to 60° C. under stirring, and the reaction was stirred at this temperature for 10 hours.
[0040] After the reaction, the resulting mixture was naturally cooled to room temperature, and fully washed with water 2-3 times, and the organic layer was separated; the organic layer was concentrated under reduced pressure to obtain a residue, which was eluted and separated by 300-400 mesh silica gel column chromatography, and A mixture of ethyl acetate and acetone with a volume ratio of 1:2 was used as the eluent to obtain the compound of the above formula (IV) with a yield of 96.1%.
[0041] 1 H-NMR (400MHz, CDCl3 )δ: 7.82(s, 1H), 7.24(d, J=4.0Hz, 2H), 7.15(dt, J=8.5, 4.3Hz,...
Embodiment 2
[0044]
[0045] At room temperature, add 100mmol of the above formula (I) compound, 150mmol of the above formula (II) compound, 150mmol of the above formula (III) compound, 3mmol [Pd(CH 3 EN) 4 ](BF 4 ) 2 , 30mmol 1-ethyl-3-methylimidazolium dicyanamide salt and 400mmol DAB CO, the temperature was raised to 80°C under stirring, and the reaction was stirred at this temperature for 8 hours.
[0046] After the reaction, the resulting mixture was naturally cooled to room temperature, and fully washed with water 2-3 times, and the organic layer was separated; the organic layer was concentrated under reduced pressure to obtain a residue, which was eluted and separated by 300-400 mesh silica gel column chromatography, and A mixture of ethyl acetate and acetone with a volume ratio of 1:3 was used as the eluent to obtain the compound of the above formula (IV) with a yield of 96.7%.
[0047] 1 H-NMR (00MHz, CDCl 3 )δ: 7.84(s, 1H), 7.18(d, J=8.6Hz, 2H), 6.83(d, J=8.6Hz, 2H), 6.41...
Embodiment 3
[0050]
[0051] At room temperature, add 100mmol of the above formula (I) compound, 130mmol of the above formula (II) compound, 200mmol of the above formula (III) compound, 5mmol [Pd(CH 3 EN) 4 ](BF 4 ) 2 , 20mmol 1-ethyl-3-methylimidazolium dicyanamide salt and 500mmol DAB CO, the temperature was raised to 100°C under stirring, and the reaction was stirred at this temperature for 6 hours.
[0052] After the reaction, the resulting mixture was naturally cooled to room temperature, and fully washed with water 2-3 times, and the organic layer was separated; the organic layer was concentrated under reduced pressure to obtain a residue, which was eluted and separated by 300-400 mesh silica gel column chromatography, and A mixture of ethyl acetate and acetone with a volume ratio of 1:2 was used as the eluent to obtain the compound of the above formula (IV) with a yield of 96.3%.
[0053] 1 H-NMR (400MHz, CDCl 3 )δ: 7.77(s, 1H), 7.16-7.11(m, 2H), 7.05(t, J=8.6Hz, 2H), 6.82(d...
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