Preparation method of semiprotic compound and product and application of semiprotic compound
A compound and organic compound technology, applied in the field of compound preparation, to achieve the effect of simple product purification and simple preparation method
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Embodiment 1
[0032] Prepare the nitrate of semi-protonic compound imidazole-imidazole, concrete method is as follows:
[0033] Dissolve 1 g of white imidazole in 10 mL of water, then add excess NH 4 NO 3 Aqueous solution (NH 4 NO 3 The molar ratio with imidazole is 2:1). Stir the reaction at room temperature for 12 hours, add excess chloroform to dissolve the product after freeze-drying, and separate the product by column chromatography to obtain light brown semi-protic imidazole-imidazole nitric acid with a melting point of 174-176°C.
[0034] 1H NMR (400MHz, Deuterium Oxide): δ7.68(s, 2H), 6.39(s, 1H), 3.59(t, J=7.4Hz, 1H), 1.13(t, J=7.1Hz, 2H). HRMS: [C 6 h 9 N 4 ]NO 3 , molecular ion peak 137.2. Its structure is as follows:
[0035]
Embodiment 2
[0037] Preparation of semi-protic compound thiophene-thiophene hexafluorophosphoric acid, the specific method is as follows:
[0038] Dissolve 1 g of thiophene in 10 mL of ethanol solution, then add excess NH 4 PF 6 Alcoholic solution (wherein NH 4 PF 6 The molar ratio to thiophene is 1.5:1), mix well at room temperature, add appropriate amount of acetonitrile to dissolve the product after freeze-drying, filter the supernatant, and dry to obtain a light yellow product with a melting point of 89-91°C.
[0039] 1H NMR(400MHz,DMSO-d6):δ8.33-8.23(m,5H),8.03-7.94(m,5H),7.23(s,1H),7.10(s,1H),6.98(s,1H) . HRMS: [C 8 h 9 S 2 ]PF 6 , molecular ion peak 169.3. Its structure is as follows:
[0040]
Embodiment 3
[0042] Preparation of semi-protic compound purine-pyrimidine hexafluorophosphate, the specific method is as follows:
[0043]Dissolve 1 g of white purine and white pyrimidine (the molar ratio of purine to pyrimidine is 1:1) in 10 mL of water, stir at room temperature for 2 h, and then add NH with a molar ratio of 3:1 4 PF 6 Aqueous solution (where NH 4 PF 6 The molar ratio to purine is 3:1), after lyophilization, add an appropriate amount of acetonitrile to dissolve the product, filter the supernatant, and dry to obtain light yellow semi-protic purine-pyrimidine hexafluorophosphate, with a melting point of 228-230°C.
[0044] 1H NMR (400MHz, Deuterium Oxide) δ9.10(d, J=1.9Hz, 1H), 8.92(s, 1H), 8.57(s, 1H), 4.74(s, 8H), 4.63(s, 5H). HRMS: [C 9 h 9 N 6 ]PF 6 , molecular ion peak 201.2. Its structure is as follows:
[0045]
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