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Comanthus parvicirrus ( 小卷海齒花 )

Comanthus parvicirrus ( 小卷海齒花 ). 動物界 (Animalia) 棘皮動物門 (Echinodermata) 海百合綱 (Crinoidea) 關節亞鋼 (Articulata) 海羊齒目 (Comatulida) 櫛羽星科 (Comasteridae). 為一種始見於石炭紀的 棘皮動物 ，生活於海裡， 具多條腕足，身體呈花狀，錶面有石灰質的殼。 常棲息於 岩縫、石、軟珊瑚的基部 。. 抽取與分離. General Experimental Procedures.

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Comanthus parvicirrus ( 小卷海齒花 )

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  1. Comanthus parvicirrus (小卷海齒花) 動物界 (Animalia) 棘皮動物門 (Echinodermata) 海百合綱 (Crinoidea) 關節亞鋼 (Articulata) 海羊齒目 (Comatulida) 櫛羽星科 (Comasteridae) 為一種始見於石炭紀的棘皮動物，生活於海裡， 具多條腕足，身體呈花狀，錶面有石灰質的殼。 常棲息於岩縫、石、軟珊瑚的基部。

  2. 抽取與分離

  3. General Experimental Procedures. • UV spectra were measured in MeOH on a Perkin-Elmer Lambda 15 UV/vis spectrometer. • IR spectra were recorded on an ATI Mattson Genesis FTIR, using KBr discs. • 1H, 13C, and all other NMR 2D experiments were recorded in CDCl3, either on a Varian Unity INOVA 400 MHz spectrometer or on a Bruker Avance 600 MHz spectrometer with a cryoprobe. • TMS was used as an internal reference for the 1H NMR spectra, and the CDCl3 signal at 77.0 ppm was used as a reference for 13C NMR spectra. • ESIMS was carried out on a Perseptive Biosystem Mariner LC-MS. • HRESIMS analysis was carried out at the EPSRC National Mass Spectrometry Service Centre in Swansea (UK). • HPLC separations were carried out using a Phenomenex reversed-phase (C18, 10 × 250 mm, 5 μm) • HPLC column and an HP1100 HPLC system (Agilent Technologies) with a diode array detector (DAD).

  4. 抽取與分離 MeOH extract of C. parvicirrus (1.1g dry weight) Partitioned by H2O-CH2Cl2 fractionation H2O-soluble CH2Cl2-soluble Hexanes/10%MeOH Partitione 50% MeOH-soluble Extracted with CH2Cl2 CH2Cl2-soluble Reversed-phase HPLC Compound 1 (61 mg) Compound 2 (34 mg)

  5. naphthopyrones 6-methoxycomaparvin (1) 6-methoxycomaparvin 5-methyl ether (2)

  6. 結構解析

  7. naphthopyrones 6-methoxycomaparvin (1) brown needle-shaped crystals UV (MeOH) λmax (logε) 245 (4.57), 290 (4.37), 380 (3.77) nm IR (KBr) νmax 3341, 2950, 1667, 1615, 1571, 1537, 1448 cm-1 LRESIMS m/z 331 [M + H]+ (C18H18O6) HRESIMS m/z 331.1176 [M + H]+, (calc for C18H19O6) 1H NMR (400 MHz, CDCl3) δ: 1.8 (2H, m, H-12) Methylene (CH2) 1.01 (3H, t, H-13) 6.23 (2H, t J=7.7 Hz, H-11) Methyl (CH3) 3.94 (3H, s, H-16) 6.23 (1H, s, H-3) Methine (CH) 6.43 (1H, d, J=1.6 Hz, H-9) 12.90 (s, OH-5) 7.01 (1H, d, J=1.6 Hz, H-7) 3.95 (3H, s, H-15)

  8. 13C NMR : 20.0 (C-12) 13.7 (C-13) 36.5 (C-11) 56.2 (C-16) 170.1 (C-2) 109.5 (C-3) 152.4 (C-10b) 136.1 (C-10a) 183.4 (C-4) 160.2 (C-10) 96.7 (C-9) 147.1 (C-4a) 104.9 (C-8) 109.3 (C-5) 134.7 (C-6) 96.3 (C-7) 158.3 (C-6a) 60.4 (C-15)

  9. HMBC

  10. COSY

  11. single-crystal X-ray diffraction analysis

  12. 6-methoxycomaparvin 5-methyl ether (2) brown needle-shaped crystals UV (MeOH) λmax (logε) 240 (4.58), 280 (4.51), 365 (4.05) nm IR (KBr) νmax 3229, 2960, 1642, 1584, 1415 cm-1 LRESIMS m/z 345 [M + H]+ (C19H20O6) HRESIMS m/z 345.1337 [M + H]+, (calc for C19H21O6) 1H NMR (400 MHz, CDCl3) δ: 12.90 (s, OH-5) 3.93 (s, H-14) 6-methoxycomaparvin 5-methyl ether (2) naphthopyrones 6-methoxycomaparvin (1)

  13. 13C NMR : 62.0 (C-14) 6-methoxycomaparvin 5-methyl ether (2) naphthopyrones 6-methoxycomaparvin (1)

  14. HMBC

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