空桐树的化学成分研究

Vol 20HUANGPing,etal:ChemicalConstituentsintheHeartwoodofPaulowniakawakamii

273

Hz,H 11),1.83(2H,,tJ=6.6Hz,H 12),1.61

13

(6H,s,H 14andH 15);http://doc.wendoc.compachol(3)

KBr

1

[8,12]

(C 5 ),107 6(C 2),107 1(C 2 ),101 5( O CH2 O ),101 3( O CH2 O ),91 9(C 8),87 7

(C 7),86 0(C 7 ),75 0(C 9),71 8(C 9 ),60 6(C 8 )

Sitosterylplamitate(6) Whiteamorphous

KBr 1

powder IR m:3426,1738,1466,1416,1381,maxc1177,722;APCI MSm/z(rel int ):397[M+H C16H32O2](100);HNMR#:5 38(1H,d,J=4 7Hz,H 6),4 62(1H,m,H 3),2 32(2H,d,J=7 3Hz,H 4),2 27(2H,,tJ=7 5Hz,H 2 ),2 01(1H,m,Hb 12),1 98(1H,m,Hb 7),1 86(1H,m,Hb 1),1 85(1H,m,H 2),1 67(1H,m,H 25),1 61(6H,m,H 15,H 16andH 3 ),1 58(1H,m,H 2),1 56(1H,m,H 7a),1 50(2H,m,H 11),1 45(1H,m,H 8),1 37(1H,m,H 20),1 29(28H,m,H 4 H 15 ,H 22,H 28),1 16(3H,m,Ha 12andH 23),1 15(1H,m,Ha 1),1 12(1H,m,H 17),1 03(3H,s,H 19),1 02(1H,m,H 14),0 94(1H,m,H 24),0 93(3H,d,J=6 4Hz,H 21),0 93(1H,m,H 9),0 89(3H,,tJ=6 8Hz,H 16 ),0 86(3H,,tJ=7 4Hz,H 29),0 85(3H,d,J=7 0Hz,H 26),0 83(3H,d,H 27),0 69(3H,s,H 18);

13

+

1

[6,17]

Yellowneeds(MeOH),

mp 138 140#;UV(MeOH)!,276;maxnm:202,252IR m:3354,1641,1591,1369,1272,1239,maxc1153,937,845,724;APCI MSm/z(rel int ):243

+1

[M+H](100);HNMR#:8 13(1H,dd,J=7 6Hz,H 8),8 07(1H,dd,J=7 6Hz,H 5),7 75(1H,td,J=7 6,1 6Hz,H 7),7 71(1H,td,J=7 6,1 6Hz,H 6),7 32(1H,s,3 OH),5 22(1H,t,tJ=7 3,1 3Hz,H 12),3 27(2H,d,J=7 3Hz,

13

H 11),1 80(3H,s,H 15),1 69(3H,s,H 14);CNMRdataseeTable1

Sesamin(4) Colourlessneeds(MeOH),mp122 124#;UV(MeOH)!,287;maxnm:207,237IR m:2968,1042,1315,1135,954,750;ESI MSmaxcm/z(rel int ):377[M+Na]

+

KBr

1

[13,14]

(100);HNMR#:

1

6 86(2H,d,J=1 4Hz,H 2andH 2 ),6 81(2H,dd,J=8 1,1 5Hz,H 6andH 6 ),6 78(2H,d,J=7 9Hz,H 5andH 5 ),5 95(4H,s, O CH2 O ),4 72(2H,d,J=4 4Hz,H 7andH 7 ),4 24(2H,dd,J=9 2,2 3Hz,Ha 9andHa 9 ),3 88(2H,dd,J=9 3,3 7Hz,Hb 9andHb 9 ),3 06(2H,m,H 8andH 8 );CNMR#:148 2(C 4andC 4 ),147 3(C 3andC 3 ),135 3(C 1andC 1 ),119 5(C 6andC 6 ),108 4(C 5andC 5 ),106 7(C 2andC 2 ),101 3( O CH2 O ),86 0(C 7andC 7 ),71 9(C 9andC 9 ),54 5(C 8andC 8 )

Paulownin(5) Colourlessneeds(MeOH),mp 105 107#:UV(MeOH)!,287;maxnm:207,237IR m:3452,2870,1493,1444,1255,1037,934,maxc811;ESI MSm/z(rel int ):393[M+Na]

1

+

KBr

1

[14 16]

13

C

NMR#:173 6(C 1 ),140 0(C 5),122 8(C 6),

73 9(C 3),56 9(C 14andC 17),50 3(C 9),46 1(C 4),42 4(C 13),40 0(C 12),38 4(C 4),37 3(C 1),36 8(C 10),36 4(C 20),35 0(2 ),34 2(C 22),32 1(C 7andC 8),29 3 29 9(C 4 14 ),29 4(C 25),28 5(C 2),28 1(C 16),26 4(C 23),25 3(C 3 ),24 5(C 15),23 3(C 28),22 9(C 15 ),21 3(C 11),20 0(C 26),19 6(C 19),19 3(C 27),19 0(C 21),14 3(C 16 ),12 2(C 29),12 1(C 18).

Hydrolysisof6

Asolutionof6(20mg)in2NNaOH MeOH(4mL)wasrefluxedfor4h.H2Owasaddedtothereactionmixture,whichwasthenextractedwithpetro.lThepet rollayerwaswashedwithH2OandconcentratedunderN2toyield http://doc.wendoc.comPCI MSm/z:415[M+H],397[M+H H2O].TheH2Olayerwasadjus tedtopH=7withHC,lthenextractwithCHCl3.Af terremovingCHCl3underN2,theresiduein2NHCl MeOH(4mL)wasrefluxedfor6h.H2Owasaddedtow+

+

(100);HNMR#:6 95(1H,d,J=1 5Hz,H 2 ),

6 92(1H,s,H 2),6 87(1H,m,H 6 ),6 85(1H,m,H 5),6 80(1H,d,J=8 0Hz,H 5 ),5 98(2Hs, O CH2 O ),5 96(2H,s, O CH2 O ),4 84(2H,J=5 0Hz,H 6andH 7 ),4 82(1H,s,H 7),4 51(1H,dd,J=9 1,0 8Hz,Hb 9 ),4 04(1H,d,J=9 4Hz,Hb 9),3 91(1H,d,J=9 4Hz,Ha 9),3 83(1H,dd,J=9 2,6 1Hz,Ha 9 ),3 04(1H,m,H 8 );CNMR#:148 4(C 4),148 2(C 4 ),148 1(C 3),147 5(C 3 ),134 8(C 1 ),129 4(C 1),36 13

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