Process control method for synthesizing 3-cyano-2, 6-dihydroxy-4-trifluoromethylpyridine triethylamine salt
A technology of trifluoromethylpyridine triethylamine salt and dihydroxy, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc., to achieve peak overlap, reduce peak interference, and improve accuracy Effect
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Embodiment 1
[0052] The reaction solution sample of 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt that has been reacted for 4 hours, the conversion rate of ethyl trifluoroacetoacetate is estimated by the synthesizer according to the synthesis process 50%, it is necessary to know the exact reaction process, and use nuclear magnetic resonance fluorine spectroscopy for detection and analysis. The specific steps include:
[0053] (1) Accurately weigh the reaction solution of internal standard 4-trifluoromethylnicotinic acid 35.79mg and 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt with a content of 98.24% 267.8mg into the sample bottle, add 0.4mL deuterated dimethyl sulfoxide to dissolve, then transfer to NMR tube for NMR detection. The sampling center frequency is -100ppm, the pulse dump angle is 90 degrees, the test temperature is 30°C, the spectral width is 237.16ppm, the delay time is 20s, the number of scans is 32 times, and the number of sampling p...
Embodiment 2
[0056] The reaction solution sample of 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt that has been reacted for 16 hours, the conversion rate of ethyl trifluoroacetoacetate is estimated by the synthesizer according to the synthesis process About 80%, it is necessary to know the accurate reaction process, and use nuclear magnetic resonance for detection and analysis. The specific steps include:
[0057] (1) Accurately weigh 25.78 mg of internal standard N-methyl-N-(trimethylsilyl) trifluoroacetamide, 3-cyano-2,6-dihydroxy-4-trifluoroacetamide with a content of 97.50% Add 310.2 mg of the reaction solution of picoline triethylamine salt to a sample bottle, add 0.4 mL of deuterated methanol to dissolve it, and transfer it to an NMR tube for NMR detection. The sampling center frequency is -100ppm, the pulse dump angle is 90 degrees, the test temperature is 30°C, the spectral width is 237.16ppm, the delay time is 20s, the number of scans is 32 times, and the numb...
Embodiment 3
[0060] The existing reaction solution sample of 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt, which has been reacted for 24 hours, needs to know the exact reaction process, and use nuclear magnetic resonance for detection and analysis. Steps include:
[0061] (1) Accurately weigh 315.20 mg of the internal standard ciprofloxacin 13.10 mg and 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt to the sample In the bottle, add 0.4mL deuterated dimethyl sulfoxide to dissolve and transfer to NMR tube for NMR detection. The sampling center frequency is -100ppm, the pulse dump angle is 90 degrees, the test temperature is 30°C, the spectral width is 237.16ppm, the delay time is 20s, the number of scans is 32 times, and the number of sampling points is 64K.
[0062] (2) if image 3 As shown, in the fluorine spectrum, the chemical shift is the quantitative peak of 3-cyano-2,6-dihydroxy-4-trifluoromethylpyridine triethylamine salt at δ=64.59ppm; the...
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