Structural elucidation of lemonomycin, a potent antibiotic from Streptomyces candidus

Author:

He Haiyin,Shen Bo,Carter Guy T

Publisher

Elsevier BV

Subject

Organic Chemistry,Drug Discovery,Biochemistry

Reference9 articles.

1. Whaley, H. A.; Patterson, E. L.; Dann, M.; Shay, A. J.; Porter, J. N. Antimicrob. Agents Chemother. 1964, 8, 83–86.

2. Chopra, I. J.; Hodgson, B. M.; Poste, G. Antimicrob. Agents Chemother. 1997, 41, 497–503.

3. [α]D=−128° (c 0.23, H2O); HR-ESI-MS m/z 552.2910 (MH+, 10%, C27H42N3O9 requires: 552.2915), 276.6494 (MH22+, 100%); UV λmax (MeOH, HP1100 diode array detector) 272, 362 nm; IR νmax (KBr) cm−1 3403, 2942, 1655, 1600, 1465, 1451, 1381, 1347, 1234.

4. The absolute stereochemistry of lemonomycin has not been determined experimentally, but the configuration of the aglycon was depicted according to the absolute stereochemistry of the isoquinoline antibiotics, saframycins (Ref. 6).

5. A solution of lemonomycin (1, 25 mg) in isopropanol (1 ml), DMSO (0.5 ml), and trifluoroacetic acid (TFA, 15 ul) was stirred at rt for 16 h. The reaction mixture was then chromatographed by HPLC on a C18 column (5 μm, 30×250 mm), using a gradient solvent of 8–30% MeCN in water (0.05% formic acid) over 17 min (20 ml/min). The UV peak at 15 min was collected (25 ml), which contained compound 2. ESI-MS m/z 618.2 (MH+), UV λmax (0.01% TFA in MeCN/H2O, diode array detector) 272, 362 nm. To this solution, NaCN (30 mg) was added, and the resulting mixture was stirred for 15 h. The solution was then evaporated in vacuo, and the residue was separated by HPLC (C18 column, 15–30% MeCN in water (0.05% formic acid)) to afford 3 (10.2 mg, 40% overall yield). ESI-MS m/z 645.4 (MH+); UV λmax (0.01% TFA in MeCN/H2O, diode array detector) 272, 362 nm; 1H NMR (CD3OD) δ 4.88 (br d, 4.5 Hz, H-1′), 4.52 (d, 3.8 Hz, H-16), 4.04 (d, 2.5 Hz, H-17), 3.99 (3H, OCH3), 3.91 (m, H-5′), 3.89 (m, H-1), 3.78 (2H, m, CH’s on isopropoxy’s), 3.72 (dd, 10.2, 3.6 Hz, H-18), 3.71 (m, H-13), 3.53 (dd, 10.2, 1.5 Hz, H-18), 3.29 (m, H-11), 2.73 (br d, 10.5 Hz, H-3), 2.67 [6H, s, N(CH3)2], 2.66 (m, H-4), 2.36 (m, H-15), 2.20 (d, 1.8 Hz, H-4′), 2.02 (dd, 17.0, 2 Hz, H-4), 1.92 (3H, s, CH3-6), 1.85 (m, H-2′), 1.78 (2H, m, H2-14), 1.67 (br d, 14.4 Hz, H-2′), 1.30 (3H, d, 6.9 Hz, H3-6′), 1.17 (3H, s, CH3-3′), 1.11-1.18 (12H, m, CH3’s on isopropoxy’s).

同舟云学术

1.学者识别学者识别

2.学术分析学术分析

3.人才评估人才评估

"同舟云学术"是以全球学者为主线,采集、加工和组织学术论文而形成的新型学术文献查询和分析系统,可以对全球学者进行文献检索和人才价值评估。用户可以通过关注某些学科领域的顶尖人物而持续追踪该领域的学科进展和研究前沿。经过近期的数据扩容,当前同舟云学术共收录了国内外主流学术期刊6万余种,收集的期刊论文及会议论文总量共计约1.5亿篇,并以每天添加12000余篇中外论文的速度递增。我们也可以为用户提供个性化、定制化的学者数据。欢迎来电咨询!咨询电话:010-8811{复制后删除}0370

www.globalauthorid.com

TOP

Copyright © 2019-2024 北京同舟云网络信息技术有限公司
京公网安备11010802033243号  京ICP备18003416号-3