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1342284605
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note
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2O). Compound 1, 2, coeluting in the analytical HPLC, and 4 were separated by HSCCC yielding pure compound 1 (6 mg) and a mixture of compounds 2 and 4 (37 mg, >95% 2). Compound 3 was further purified by preparative HPLC (3 mg) from another HSCCC fraction.
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19
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1342305781
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note
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(b) HPLC: HP 1100 liquid Chromatograph (stationary phase, Zorbax SB-C-18 (150 x 4.6 mm, 3.5 μm); mobile phase, solvent A water, solvent B acetonitril; gradient O min 80% A, 22 min 60% A, 40 min 20% A) equipped with a diode array detector (detection at 200, 230, and 267 nm) and operating at room temperature.
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20
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1342263286
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note
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(c) HPLC-MS: coupling of the HPLC system described above to a Bruker Esqire 3000plus (ion source ESI, negative mode; spray voltage 4500 V; nebulizer gas N2, 40 psi; dry gas N2, 10 L/min, 350°C). The HPLC setup was equal to the HPLC-DAD method, only solvent A was replaced by 0.15% acetic acid.
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1342263288
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3 solution at 300 K. All signals were unambiguously assigned by using 2D correlation data (DQF-COSY, HSQC, HMBC, ROESY).
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1342263290
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note
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2-22 with H-23.
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1342263289
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3-27.
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