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20xx年婦科千金方化學(xué)成分的研究(編輯修改稿)

2025-01-25 22:21 本頁面
 

【文章內(nèi)容簡介】 C7) , (C8) , (C9) , (C10) , (C11) , (C12) , (C13) , (C14) , (C15) , (C16) , (C17) , (C18) , (C19) , (C20) .NMR數(shù)據(jù)與文獻(xiàn)[2930]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物11為穿心蓮內(nèi)酯。
  
  化合物12無色針狀結(jié)晶 (Me OH) , mp 203~204℃;EIMS m/z 332[M]。HNMR (pyridined5, 400MHz) δ: (1H, m, Ha1) , (1H, m, Hb1) , (2H, m, H22) , (1H, dd, J=, Hz, H3) , (1H, dd, J=, Hz, H5) , (1H, m, Ha6) , (1H, br dd, J=, Hz, Hb6) , (2H, m, H27) , (1H, d, J= Hz, H9) , (1H, dd, J=, Hz, H11) , (1H, d, J= Hz, H12) , (1H, br t, J= Hz, H14) , (2H, br d, J= Hz, H215) , (1H, br s, Ha17) , (1H, br s, Hb17) , (3H, s, H318) , (1H, d, J= Hz, Ha19) , (1H, d, J= Hz, Hb19) , (3H, s, H320) , (1H, s, 3OH) , (1H, s, 19OH) 。CNMR (pyridined5, 100 MHz) δ: (C1) , (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C11) , (C12) , (C13) , (C14) , (C15) , (C16) , (C17) , (C18) , (C19) , (C20) .NMR數(shù)據(jù)與文獻(xiàn)[31]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物12為脫水穿心蓮內(nèi)酯。
  
  化合物13無色針狀結(jié)晶 (Me OH) , mp 210~211℃;EIMS m/z 350[M]。HNMR (pyridined5, 400MHz) δ: (1H, m, Ha1) , (1H, m, Hb1) , (2H, m, H22) , (1H, dd, J=, Hz, H3) , (1H, dd, J=, Hz, H5) , (1H, m, Ha6) , (1H, qd, J=, Hz, Hb6) , (2H, m, H27) , (1H, dd, J=, Hz, H9) , (1H, dd, J=, Hz, Ha11) , (1H, ddd, J=, , Hz, Hb11) , (1H, br t, J= Hz, H12) , (1H, br s, H14) , (1H, dd, J=, Hz, Ha15) , (1H, dd, J=, Hz, Hb15) , (1H, br s, Ha17) , (1H, br s, Hb17) , (3H, s, H318) , (1H, d, J=, Ha19) , (1H, br d, J= Hz, Hb19) , (3H, s, H320) 。CNMR (pyridined5, 100 MHz) δ: (C1) , (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C11) , (C12) , (C13) , (C14) , (C15) , (C16) , (C17) , (C18) , (C19) , (C20) .NMR數(shù)據(jù)與文獻(xiàn)[31]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物13為異穿心蓮內(nèi)酯。
  
  化合物14黃色粉末;EIMS m/z 328[M]。HNMR (CDCl3, 400 MHz) δ: (1H, s, H3) , (1H, s, H6) , (1H, dd, J=, Hz, H3’) , (1H, td, J=, , Hz, H4‘) , (1H, dd, J=, Hz, H5’) , (1H, dd, J=, Hz, H6‘) , (3H, s, 7OMe) , (3H, s, 8OMe) , (3H, s, 2’OMe) , (1H, br s, 5OH) .NMR數(shù)據(jù)與文獻(xiàn)[32]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物14為穿心蓮黃酮。
  
  化合物15黃色粉末;EIMS m/z 284[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, s, H6) , (1H, s, H8) , (2H, d, J= Hz, H2’, 6’) , (2H, d, J= Hz, H3’, 5‘) , (3H, s, 4’OMe) , (1H, s, 5OH) , (1H, s, 7OH) 。CNMR (DMSOd6, 100 MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1’) , (C2’, 6‘) , (C3’, 5’) , (C4‘) , (OMe) .NMR數(shù)據(jù)與文獻(xiàn)[33]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物15為鷹嘴豆芽素A.
  
  化合物16黃色針狀結(jié)晶 (三氯甲烷) , mp195~197176。C。EIMS m/z 358[M]。HNMR (CDCl3, 400 MHz) δ: (1H, s, H3) , (1H, s, H6) , (1H, d, J= Hz, H3’) , (1H, dd, J=, Hz, H4‘) , (1H, d, J= Hz, H6’) , (3H, s, 7OMe) , (3H, s, 8OMe) , (3H, s, 2’OMe) , (3H, s, 5’OMe) , (5OH) 。CNMR (CDCl3, 100 MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1‘) , (C2’) , (C3‘) , (C4’) , (C5‘) , (C6’) , (7OMe) , (8OMe) , (2’OMe) , (5’OMe) .NMR數(shù)據(jù)與文獻(xiàn)[34]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物16為5羥基7, 8, 2’, 5’四甲氧基黃酮。
  
  化合物17白色粉末;EIMS m/z 268[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, d, J= Hz, H5) , (1H, dd, J=, Hz, H6) , (1H, d, J= Hz, H8) , (2H, d, J= Hz, H2’, 6‘) , (2H, d, J= Hz, H3’, 5’) , (3H, s, 4’OMe) , (1H, br s, 7OH) 。CNMR (DMSOd6, 100MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1‘) , (C2’, 6’) , (C3’, 5‘) , (C4’) , (OMe) .NMR數(shù)據(jù)與文獻(xiàn)[6]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物17為芒柄花素。
  
  化合物18白色粉末;EIMS m/z 254[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, d, J= Hz, H5) , (1H, dd, J=, Hz, H6) , (1H, d, J= Hz, H8) , (2H, d, J= Hz, H2’, 6‘) , (2H, d, J= Hz, H3’, 5’) , (1H, s, 7OH) , (1H, s, 4’OH) 。CNMR (DMSOd6, 100 MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1‘) , (C2’, 6’) , (C3’, 5‘) , (C4’) .NMR數(shù)據(jù)與文獻(xiàn)[6, 33]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物18為大豆苷元。
  
  化合物19白色粉末;EIMS m/z 270[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, br s, H6) , (1H, br s, H8) , (2H, d, J= Hz, H2’, 6‘) , (2H, d, J= Hz, H3’, 5’) , (1H, s, 5OH) 。CNMR (DMSOd6, 100 MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1‘) , (C2’, 6’) , (C3’, 5‘) , (C4’) .NMR數(shù)據(jù)與文獻(xiàn)[6]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物19為染料木素。
  
  化合物20無色晶體 (Me OH) 。EIMS m/z 122[M]。HNMR (DMSOd6, 400 MHz) δ: (2H, d, J= Hz, H2, 6) , (2H, t, J= Hz, H3, 5) , (1H, t, J= Hz, H4) 。CNMR (DMSOd6, 100 MHz) δ: (C1) , (C2, 6) , (C3, 5) , (C4) , (COOH) .NMR數(shù)據(jù)與文獻(xiàn)[35]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物20為苯甲酸。
  
  化合物21白色粉末;EIMS m/z 168[M]。HNM R (400 MHz, DMSOd6) δ: (1H, br s, H2) , (1H, d, J= Hz, H5) , (1H, br d, J= Hz, H6) , (3H, s, OMe) , (1H, s, COOH) 。CNMR (400 MHz, DMSOd6) δ: (C1) , (C2) , (C3) , (C4) , (C5) , (C6) , (OMe) , (COOH) .NMR數(shù)據(jù)與文獻(xiàn)[36]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物21為香草酸。
  
  化合物22淡黃色針狀結(jié)晶 (水) , mp 172~173℃;EIMS m/z 194[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, d, J= Hz, H5) , (1H, d, J= Hz, H6) , (1H, d, J= Hz, H7) , (1H, d, J= Hz, H8) , (3H, s, OMe) , (1H, s, COOH) 。CNMR (DMSOd6, 100 MHz) δ: (C1) , (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (OMe) , (COOH) .NMR數(shù)據(jù)與文獻(xiàn)[22]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物22為反式阿魏酸。
  
  化合物23白色粉末;EIMS m/z 138[M]。HNMR (DMSOd6, 400 MHz) δ: (1H, d, J= Hz, H3) , (1H, td, J=, Hz, H4) , (1H, td, J=, Hz, H5) , (1H, dd, J=, Hz, H6) , (1H, br s, COOH) 。C NMR (DMSOd6, 100 MHz) δ: (C1) , (C2) , (C3) , (C4) , (C5) , (C6) , (COOH) .NMR數(shù)據(jù)與文獻(xiàn)[35]報(bào)道的數(shù)據(jù)對(duì)比, 鑒定化合物23為水楊酸。
  
  化合物24白色粉末;ESIMS m/z 415[M–H]。HNMR (DMSOd6, 400 MHz) δ: (1H, s, H2) , (1H, d, J= Hz, H5) , (1H, dd, J=, Hz, H6) , (1H, d, J= Hz, H8) , (2H, d, J= Hz, H2’, 6‘) , (2H, d, J= Hz, H3’, 5’) , (1H, d, J= Hz, H1”) , – (4H, m, 2“H–5”H) , (1H, dd, J=, Hz, Ha6“) , (1H, dd, J=, Hz, Hb6”) , (1H, s, 4’OH) 。CNMR (DMSOd6, 100 MHz) δ: (C2) , (C3) , (C4) , (C5) , (C6) , (C7) , (C8) , (C9) , (C10) , (C1‘) , (C
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