求职-2013年工作汇报的化学成分研究

69-XY2-69-1/未新269-苯丙糖接正丁醇的工产已归//新78-不只有谱////78-梫木素木藜XVIII已归////79-不只有谱////86-苯丙糖不////89-木藜XVIII-糖已归/根确新89-小分不///591-木脂糖不////594-萜糖两个已已归/已95-单萜苷文献只面构已归/未定已595-XY3-30-已归///5XY3-5木脂糖还没解////XY3-1不////2XY3-4小分糖两个五元环合糖已归/未定新3XY3-5苯丙糖两个混合物不////3XY3-4苯丙糖不////XY3-6小分不////XY3-3降倍萜糖混合物，不////3XY3-4不////311-不///13-小分不只有谱///216-有二萜，量少，无法富///118-萜，HPLC法富///218-萜糖已知eA已归//524-降倍萜糖谱图不///324-降倍萜糖XY3-18-重已归///25-两个二萜混HPLC///26-降倍萜糖两个构型异混合///526-降倍萜糖苷元已知的糖已归/未定/30-已知已归/根确/32-小分不///132-已知ideB已归///31、化合物极性较大，正相硅分离效果不好，常有吸附，2、运用反相ODSTLC难以检测，必须浓缩3、由于化合物基本上都为糖苷，分子量差别不是很大，故凝4、HPLCTLC上显示为一个HPLC纯化仍然有许多杂峰，分离度欠佳。（60°C，导致不稳定的化合物变性，使得后续的分离工作重重。二、化合物数据汇总1、XY2-67-3已知化合物2,3-dihydro-2-(4'-hydroxy-3'-methoxypheny1)-3-hydroxymethy1-7-methoxy-5-(3-O-α-rham NMRNMRNMRspetraldataofXY2-67-31H-1/C/C26.95(d,J=1.6Hz,6.71(d,J=3.4Hz,3/C/C3'-3.84(s,3-3.81(s,4/C/C56.77(d,J=8.1Hz,/C66.83(dd,J=8.1,1.76.72(d,J=3.4Hz,75.49(d,J=6.4Hz,2.64(m,83.48(dd,J=12.3,Hz,1.88(m,93.82(overlapped,3.66(m,1H)3.384.66(d,J=1.2Hz,3.853.39(m,3.61(m,3.71(m,1.23(d,J=6.2Hz,a1H-NMRDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.b13C-NMRDataweremeasureedinCD3ODat100MHz.Chemicalshifts(δ)areexpressedinppm.Obata,T.;Sawabe,A.;Morita,M.;Yamashita,N.;Matsubara,Y.,TerpenoidandphenylpropanoidglycosidesisolatedfromleavesofHiba(ThujopsisdolabrataSEIB.etZUCC.).NihonYukagakkaishi1997,46,(2),139-144.2、XY2-69-1NMRNMRspetraldataofXY2-67-31H-1//26.95(d,J=1.6Hz,6.71(d,J=3.4Hz,3/C/C3'-3.84(s,-3-3.81(s,-4/C/C56.77(d,J=8.1Hz,/66.83(dd,J=8.1,1.7Hz,6.72(d,J=3.4Hz,74.35(d,J=6.4Hz,2.64(m,83.48(dd,J=12.3,6.2Hz,1.88(m,93.82(overlapped,-3.66(m,1H)3.38(m,-4.66(d,J=1.2Hz,3.853.39(m,3.61(m,3.71(m,1.23(d,J=6.2Hz,a1H-NMRDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.b13C-NMRDataweremeasureedinCD3ODat100MHz.Chemicalshifts(δ)areexpressedinppm.3、XY2-69-5新化合物NMRNMRspetraldataofXY2-69-51H-1/4/72.86(t,J=7.5Hz,82.59(t,J=7.5Hz,9/4.04(t,J=6.5Hz,1.57(m,7.13(d,J=8.3Hz,1.34(m,7.01(d,J=8.3Hz,0.92(t,J=7.4Hz,4.85(overlapped,3.42(m,3.41(m,3.44(m,3.43(m,3.88(d,J=12.0Hz,1H)3.70(dd,J12.0,4.8Hz,a1H-NMRDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.b13C-NMRDataweremeasureedinCD3ODat100MHz.Chemicalshifts(δ)areexpressedinppm.4、XY2-89-4新化合物NMRNMRspetraldataofXY2-89-4-1H-T1(a-H)2.92(t,J=9.6Hz,-2(b-H)2.33(ddd,J=14.8,10.0,7.2Hz, (a-(ddd,J=12.3,9.3,2.6Hz,-3(a-H)3.61(overlapped,-4//5//6(a-H)3.80(overlapped,-7(b-H)2.05(dd,J=14.6,4.5Hz,1H)1.44-8//92.45(t,J=6.4Hz,-5/1.58(m,1H)1.47(m,-1.72(d,J=6.6Hz,1H)1.57(m,-2.21(br.t,-1.99(dd,J=11.4,4.1Hz,1H)1.70(overlapped,-2.04(overlapped,1H)1.71(overlapped,-//1.40(s,-1.02(s,-1.17(s,-65.04(s,1H)4.92(s,24.30(d,J=7.8Hz,-23.12(t,J=8.8Hz,-33.36(overlapped,-43.28(s,-53.23(dd,J=5.3,2.1Hz,-3.81(dd,J=11.6,2.0Hz,1H)3.64(dd,J=12.0,5.6-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.5、XY2-94-1构型尚未能确定。但无论是R,还是S构型，均已被。NMRNMRNMRspetraldataofXY2-94-1n-1H-T1/C21.92(ddd,J=12.2,3.4,2.2Hz,1H)1.57(t,=12.2Hz,-34.13(m,42.42(m,1H)2.10(m,-5/C6/C72.36(m,1H)2.29(m,-82.61(m,-9/C2.21(s,-1.70(s,-1.12(s,-1.12(s,-Glu-4.49(d,J=7.8Hz,-Glu-3.23(dd,J=8.0,1.0Hz,-Glu-3.43(m,-Glu-3.36(br.s,-Glu-3.35(m,-Glu-3.93(dd,J=11.6,2.0Hz,1H)3.75(dd,J11.9,5.1Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.Matsushita,H.;Miyase,T.;Ueno,A.,LignanandterpeneglycosidesfromEpimediumsagittatum.Phytochemistry1991,30,(6),2025-2027.6、XY2-95-3化合物名称：Uroterpenolβ-D-glucosideNMRNMRspetraldataofXY2-95-3-1H-1/C21.92(ddd,J=12.2,3.4,2.2Hz,1H)1.57(t,=12.2Hz,-34.13(m,42.42(m,1H)2.10(m,-5/C6/C72.36(m,1H)2.29(m,-82.61(m,-9/C2.21(s,-1.70(s,-1.12(s,-1.12(s,-14.49(d,J=7.8Hz,-O23.23(dd,J=8.0,1.0Hz,-33.43(m,-43.36(br.s,-53.35(m,-63.93(dd,J=11.6,2.0Hz,1H)3.75(dd,J11.9,5.1Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.Yamamura,S.;Ozawa,K.;Ohtani,K.;Kasai,R.;Yamasaki,K.,AntihistaminicflavonesandaliphaticglycosidesfromMenthaspicata.Phytochemistry1998,48,(1),131-136.7、XY3-3-4新化合物NMRNMRspetraldataofXY3-3-4-1H-T15.21(d,J=6.7Hz,22.18(m,-31.84(m,1H)1.41(m,-42.85(dd,J=14.8,7.2Hz,-52.17(m,1H)1.44(m,-6/77.49(d,J=1.1Hz,81.96(dd,J=13.3,6.7Hz,-3.56(ddd,J=27.6,10.7,6.5Hz,2/3.71(s,-4.68(d,J=7.7Hz,-23.18(t,J=8.3Hz,-33.32(overlapped,-43.30(m,-53.24(dd,J=5.3,2.0Hz,-3.89(dd,J=11.8,2.1Hz,1H)3.68(dd,J=5.2Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.8、XY3-18-5已知化合物化合物名称：LinarionosideANMRNMRspetraldataofXY3-18-5-1H-1/C21.83(ddd,J=12.0,3.6,2.4Hz,1H)1.49(t,J12.0Hz,-34.07(m,-42.42(m,1H)2.10(m,-5/C6/C72.36(m,1H)2.29(m,-82.61(m,-93.73(m,C1.19(d,J=6.2Hz,-1.07(s,-1.08(s,-1.67(s,-14.44(d,J=7.8Hz,-OCH-23.15(t,J=7.8Hz,-33.39(m,-43.32(m,-53.30(m,-63.88(dd,J=11.8,1.5Hz,1H)3.70(dd,J12.0,6.4Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.YAN,L.;XU,L.;WANG,Z.;ZHANG,Q.;YANG,S.,TwonewglycosidesfromthestemsofClematisparviloba.YaoXueXue2010,45,1527-9、XY3-26-2新化合物NMRNMRspetraldataofXY3-26-2-1H-T1/C23.21(d,J=10.0Hz,-33.92(m,-41.59(m,-5/C6/C72.30(m,1H)1.98(m,-82.28(m,1H)2.04(m,-93.71(m,C1.23(d,J=6.2Hz,-1.14(s,-0.96(s,-1.67(s,-4.38(d,J=7.8Hz,-23.19(t,J=7.8Hz,-33.39(m,-43.32(m,-53.30(m,-3.88(dd,J=11.8,1.5Hz,1H)3.71(dd,J=6.4Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.10、XY3-30-1已知化合物化合物名称：GrayanosideBNMRNMRspetraldataofXY3-30-1-1H-T1(a-H)2.94(t,J=9.5Hz,-2(b-H)2.27(ddd,J=16.4,9.7,6.9Hz, H)2.09(m,-3(a-H)3.80(overlapped,-4//5//6(a-H)3.80(dd,J=8.2,3.1Hz,-7(b-H)2.16(dd,J=14.0,10.6Hz,1H)1.30(d,J1.9Hz,-8//92.43(t,J=7.2Hz,-/1.58(m,1H)1.48(m,-1.71(d,J=14.3Hz,1H)1.57(m,-1.90(m,-1.87(m,1H)1.78(m,-1.83(m,1H)1.71(m,-//1.36(s,-1.03(s,-1.18(s,-5.01(s,1H)4.96(s,4.30(d,J=7.8Hz,-23.20(br.s-33.35(br.s,-43.29(m,-53.27(bs.s-3.86(dd,J=11.8,2.1Hz,1H)3.67(dd,J=5.2Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.;;;秦国伟,美丽马醉木化学成分的研究.中草2000,31,(6),407-11XY3-32-8NMRNMRspetraldataofXY3-32-8-1H-T12.99(t,J=10.2Hz,-2(b-H)2.21(, (a-H)1.81(m,-34.15(dd,J=9.7,4.8Hz,-4/C5//61.77-71.95(m,1H)1.30(m,-8/-92.08(dd,J=5.5,0.8Hz,-/1.70(m,1H)1.57(m,-1.77(m,--1.71-1.88(m,1H)1.60(m,-//1.36(s,-0.96(s,-1.04(s,-5.22(s,1H)5.11(s,4.28(d,J=7.7Hz,-23.18(t,J=8.3Hz,-33.32(overlapped,-43.30(m,-53.24(dd,J=5.3,2.0Hz,-3.86(dd,J=11.8,2.1Hz,1H)3.67(dd,J=5.2Hz,-aDataweremeasureedinCD3ODat400MHz.Chemicalshifts(δ)areexpressedinppm,andJvaluesarepresentedinHz.Wang,L.;Chen,S.;Cheng,K.;Li,C.;Qin,G.,DiterpeneglucosidesfromPierisformosa.Phytochemistry2000,54,(8),847-852.三、下月工作计划 3 20136XY3-33-1XY3-33-8XY3-33-2XY3-42-10II。1、XY3-39-1化合物名称：(R)-(-)-rhododendrol化合物结构化合物数据：[α]20-17.4°(c0.1,EtOH 1HNMR(400MHz,CDOD, inppm):δ1.20(1H,d,J=6.2Hz,H-10),1.69(1H,m,H-7),2.61(1H,m,H-3.74(1H,dq,J=12.5,6.2Hz,H-9),6.71(2H,d,J=8.5Hz,H-2,6),7.03(2H,d,J=8.4Hz,H-3,5);13CNMR(100MHz,CD3OD,δinppm):δ22.09(C-10),30.82(C-8),40.99(C-7),66.51(C-9),114.67(C-3,5),128.82(C-2,6),133.04(C-1),154.91(C-文献：Yuasa,Y.;Shibuya,S.;Yuasa,Y.,Resolutionofracemicrhododendrolbylipase-catalyzedenantioselectiveacetylationSyntheticcommunications2003,33,(9),1469-1475.XY3-40-3XY3-40-3化合物名称：(2R)-4-(4-hydroxy-3-methoxyphe-nyl)-2-化合物结构化合物数据：[α]D20-7.8°(c0.4,EtOH); 1HNMR(400MHz,CD3OD,δinppm):δ1.19(1H,d,J=6.2Hz,H-10),1.70(1H,m,H-7),2.60(1H,m,H-8),3.73(1H,dq,J=12.5,6.2Hz,H-9),3.83(3H,s,H-11),6.63dd,J=8.0,1.8Hz,H-6),6.70(1H,d,J=8.0Hz,H-5);6.77(1H,d,J=1.7H-2).13CNMR(100MHz,CD3OD,δinppm):δ23.54(C-10),32.71(C-7),42.35(C-8),56.35(C-11),67.59(C-9),113.14(C-2),116.09(C-5),121.72(C-6),135.21(C-1),145.89(C-4),148.84(C-文献：Yuasa,Y.;Shibuya,S.;Yuasa,Y.,Resolutionofracemicrhododendrolbylipase-catalyzedenantioselectiveacetylation.Syntheticcommunications2003,33,(9),1469-1475.XY3-40-4XY3-40-4化合化合物结构化合物数据：[α]D20+58.9°(c1.1,EtOH); 1HNMR(400MHz,CD3OD,δinppm):δ3.09(2H,m,H-8),3.79(2H,d,J=3.4Hz,H-9),3.82(6H,m,H-10),4.19(H-9,dd,J=8.9,6.8Hz,2H),4.67(2H,d,J=Hz,H-7),6.75(2H,d,J=8.1Hz,H-5),6.78(2H,d,J=8.3,1.5Hz,H-6.92(2H,d,J=1.0Hz,H-2).13CNMR(100MHz,CD3OD,δinppm):55.31(C-8),56.41(C-10),67.91(C-9),87.44(C-7),110.97(C-2),(C-5),120.03(C-6),133.78(C-1),147.26(C-4),149.07(C-Jung,HWMahesh,RLeeJ.GLeeSHKimYPark,Y.,PinoresinolfromthefruitsofForsythiakoreana toryrespon