Novel compound 6-fluoro-2,4-diamino-nitrobenzene and preparation method thereof
A technology for trifluoronitrobenzene and compounds, which is applied in the field of new compound 6-fluoro-2,4-diaminonitrobenzene and its preparation, and can solve the problem of high cost, low yield and limited fluorine-containing nitroaniline The application needs of aromatic compounds, etc., to achieve the effect of mild reaction, easy handling and purification
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Embodiment 1
[0017] The preparation method of 6-fluoro-2,4-diaminonitrobenzene of the present embodiment is as follows:
[0018] Add 67.0g (0.378mol) of 2,4,6-trifluoronitrobenzene into a 1000ml single port, and add 250mL of ethanol to dissolve, then slowly add 209g (2.646mol) of ammonium bicarbonate, after the addition is complete and mix well, at 25 After standing at ℃ for 12 hours, crystals precipitated out of the system, filtered and washed with suction, and the crude product was recrystallized with ethanol / water (v:v) = 2:1 to obtain 61.1 g of light yellow crystals, with a yield of 94.5%;
[0019] MS: m / z: [M+1]:172
[0020] 1 H NMR (400 MHz, CDCl 3 ): δ 6.24 (d, 1H), 6.10 (br, 4H), 5.92 (s, 1H)
Embodiment 2
[0022] The preparation method of 6-fluoro-2,4-diaminonitrobenzene of the present embodiment is as follows:
[0023] Add 67.0g (0.378mol) of 2,4,6-trifluoronitrobenzene into a 1000ml single port, and add 250mL of ethanol to dissolve, then slowly add 239g (3.024mol) of ammonium bicarbonate, after the addition is complete and mix well, at 25 After standing at ℃ for 10 hours, the system precipitated crystals, which were filtered and washed with suction. The crude product was recrystallized with ethanol / water (v:v) = 2:1 to obtain 59.5 g of light yellow crystals, with a yield of 92%.
Embodiment 3
[0025] The preparation method of 6-fluoro-2,4-diaminonitrobenzene of the present embodiment is as follows:
[0026] Add 67.0g (0.378mol) of 2,4,6-trifluoronitrobenzene into a 1000ml single port, and add 250mL of ethanol to dissolve, then slowly add 179g (2.268mol) of ammonium bicarbonate, after the addition is complete and mix well, at 35 After standing at ℃ for 11 hours, the system precipitated crystals, which were filtered and washed with suction. The crude product was recrystallized with ethanol / water (v:v) = 2:1 to obtain 57.6 g of light yellow crystals, with a yield of 89.2%.
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