Steroid imidazole salt compound and its preparing process
A salt compound, steroidal imidazole technology, applied in the field of novel steroidal imidazole salt compounds, can solve the problems that have not been reported in the literature
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Embodiment 1
[0029] Example 1 1-(3β-diosgenin)-3-benzyl-imidazolium bromide
[0030]
[0031] The preparation process is as follows:
[0032] The preparation of 1.1-(3β-diosgenin) imidazole compound:
[0033] Dissolve diosgenin (4.00g, 10mmol) and triethylamine (3.4ml, 24mmol) in dichloromethane solvent (400ml), stir, and slowly add methanesulfonyl chloride (1.37mg , 12mmol), after the dropwise addition was completed, the reaction was carried out at room temperature for 3 hours. After the reaction is complete, add water (50ml), neutralize with dilute hydrochloric acid, separate the organic phase, extract the aqueous phase with dichloromethane 3 times (20ml / time), combine the organic phases, and successively wash with saturated NaHCO 3 solution, washed with a saturated NaCl solution, dried over anhydrous sodium sulfate, filtered to remove the desiccant, and evaporated under reduced pressure to remove the solvent to obtain a crude product.
[0034] The above crude product (5mmol) and i...
Embodiment 2
[0041] Example 2 1-(3α-diosgenin)-3-benzyl-imidazolium bromide
[0042]
[0043] The preparation process is as follows:
[0044] 1. Preparation of 1-(3α-diosgenin) imidazole compound:
[0045] The preparation method is the same as that of compound 1 to obtain 1-(3α-diosgenin)imidazole compound with a yield of 11.5%.
[0046]2. Preparation of 1-(3α-diosgenin)-3-benzyl-imidazolium bromide:
[0047] The preparation method was the same as that of compound 1 to obtain white amorphous powder compound 2 with a yield of 94.9%.
[0048] mp.236-238℃; IR(KBr)v max cm -1 : 3435, 3063, 2950, 2873, 1631, 1558, 1455, 1377, 1242, 1134, 1052, 968, 899, 712;
[0049] ESI-MS (m / e, %): 556 ([M+1-Br] + , 43), 555 ([M-Br] + ,100);
[0050] 1 H NMR (300MHz, CDCl 3 ): δ10.18 (S, 1H), 7.54-7.51 (d, 4H), 7.38-7.36 (t, 3H), 5.73-5.68 (d, 2H, PhCH 2 ), 5.64 (S, 1H, H-6), 4.86 (S, 1H, H-3), 4.45-4.38 (dd, 1H, J=6, 15Hz), 3.49-3.34 (m, 2H), 2.95- 2.90(d, 1H, J=15Hz), 2.68-2.63(d, 1H, J=15...
Embodiment 3
[0052] Example 3 1-(3α,5α-cyclo-6β-diosgenin)-3-benzyl-imidazolium bromide
[0053]
[0054] The preparation process is as follows:
[0055] 1. Preparation of 1-(3α, 5α-ring-6β-diosgenin) imidazole compound:
[0056] The preparation method was the same as that of compound 1 to obtain 1-(3α,5α-cyclo-6β-diosgenin)imidazole compound with a yield of 37.9%.
[0057] 2. Preparation of 1-(3α, 5α-ring-6β-diosgenin)-3-benzyl-imidazolium bromide:
[0058] The preparation method was the same as that of compound 1 to obtain white amorphous powder compound 3 with a yield of 80.2%.
[0059] IR(KBr)v max cm -1 : 3432, 3056, 2951, 2850, 1631, 1558, 1454, 1381, 1217, 1053, 968, 899, 712;
[0060] ESI-MS (m / e, %): 556 ([M+1-Br] + , 41), 555 ([M-Br] + ,100);
[0061] 1 H NMR (300MHz, CDCl 3 ): δ10.92(S, 1H), 7.54-7.51(m, 4H), 7.38-7.36(m, 3H), 5.70(s, 2H, PhCH 2 ), 4.48-4.40(dd, 1H, J=9, 15Hz), 3.56(s, 1H, H-6), 3.50-3.45(dd, 1H, J=3, 12Hz), 3.41-3.34(t, 1H , J=12Hz), 2.39-2.35(d...
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