New sansanmycins, and their uses as anti-tuberculous medicines
A technology for drugs and uses, applied in the field of uridine peptide antibiotics and their preparation, can solve the problems of no anti-tuberculosis candidates with new structural skeletons, since the mid-1970s, etc.
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Embodiment 1
[0088] Embodiment 1: the synthesis of SSA-1A
[0089] Dissolve 90 mg (0.104 mmol) of 50% SSA in 2 ml of distilled water, add 20 μl of acetic anhydride (0.208 mmol), add 1 mol / L NaOH solution to adjust the pH to about 6, and stir at room temperature for 3 hours. Purified by preparative liquid chromatography to obtain 11.2 mg of white powder, yield 23.73%, ESI (-) 946.4, 1 H NMR (600M HZ, DMSO-d 6 ):δ1.72(3H,S,H N-CO-CH3 ), 2.24(3H,S,H Ar-O-CO-CH3 ), 4.73 (1H,m,H m-Tyr-2 ), 6.92 (1H, S, H m-Tyr-2‘ ), 6.94 (1H, d, J=7.2HZ, H m-Tyr-4‘ ), 6.95 (1H, d, J=7.2HZ, H m-Tyr-6‘ ), 7.01 (1H, t, J=7.2HZ, H m-Tyr-5‘ ). The remaining signals are the same as those of Sansanmycin reported in the literature (Yunying Xie, et al. The Journal of Antibiotics. 2007, 60(2): 158-161). h m-Tyr-2 The chemical shift shifted from δ3.90 to δ4.73 downfield, indicating that the free amino group was acylated; H-2', 4', 6' on m-Tyr all shifted downfield, while 5' shifted upfield The displacement indi...
Embodiment 2
[0090]Embodiment 2: the synthesis of SSA-1B
[0091] Dissolve 90mg (0.104mmol) of 50% SSA in 2ml distilled water, add 40μl acetic anhydride (0.417mmol), add 1mol / L NaOH solution to adjust the pH to about 6, and stir at room temperature for 5 hours. Purified by preparative liquid chromatography to obtain 3.5 mg of white powder, yield 7.09%, ESI (-) 988.4, 1 H NMR (600M HZ, DMSO-d 6 ):δ1.72(3H,S,H N-CO-CH3 ), 1.98 (3H,S,H R-O-CO-CH3 ), 2.24(3H,S,H Ar-O-CO-CH3 ), 4.73 (1H,m,H m-Tyr-2 ), 5.37 (1H,m,H sugar-2 ), 6.95 (1H, S, H m-Tyr-2‘ ), 6.96 (1H, d, J=7.2HZ, H m-Tyr-4‘ ), 6.97 (1H, d, J=7.2HZ, H m-Tyr-6‘ ), 7.03 (1H, t, J=7.2HZ, H m-Tyr-5‘ ). The remaining signals are the same as Sansanmycin. Like SSA-1A, the free amino group and the 3’ phenolic hydroxyl group on m-Tyr can be judged to be acylated by the change of m-Tyr signal; H sugar-2 A downfield shift indicates that the hydroxyl group on sugar-2 is acylated.
Embodiment 3
[0092] Embodiment 3: the synthesis of SSA-2
[0093] Take 50% SSA 90mg (0.104mmol) dissolved in 2ml DMSO, add 45ul triethylamine (0.312mmol), add 18ul bromoacetyl bromide (0.208mmol), stir at room temperature for 2 hours. Purified by preparative liquid chromatography to obtain 5.7 mg of white powder, yield 11.11%, ESI (-) 982.3, 984.3, 1H NMR (500M HZ, DMSO-d6): δ4.32 (2H, S, H-Br- CH2), 4.70 (1H,m,Hm-Tyr-2). The remaining signals are the same as Sansanmycin. The chemical shift of Hm-Tyr-2 shifted downfield to δ4.70, indicating that the free amino group was acylated.
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