乙酸乙酯化学成分简述.docVIP

乙酸乙酯化学成分简述 ; 用三氯甲烷-甲醇(7∶3)洗脱,最后过硅胶柱,石油醚-乙酸乙酯(8∶1)洗脱,分别得到化合物3(25mg),化合物4(30mg)。Fr.4部分过MCI柱,用85%丙酮洗脱后,经硅胶柱色谱,三氯甲烷-甲醇(20∶1,15∶1,10∶1,8∶1,6∶1)进行梯度洗脱,得到Fr.4.1~Fr.4.4,共4个部分,Fr.4.3经SephadexLH-20凝胶柱,以三氯甲烷-甲醇(5∶5)洗脱,得到化合物5(18mg)。3结构鉴定化合物1白色粉末,mp222~224℃,ESI-MSm/z221[M+H]+。1H-NMR(500MHz,CDCl3)δH:5.05(1H,d,J=2.5Hz,H-6b),4.77(1H,d,J=2.5Hz,H-6a),4.28(1H,m,H-4),2.14(1H,dt,J=11.0,6.5Hz,H-3α),2.02(1H,m,H-9β),1.99(1H,m,H-8),1.95(1H,dt,J=11.0,7.0Hz,H-2),1.83(1H,m,H-3β),1.82(1H,d,J=14.0Hz,H-12β),1.78(1H,m,H-11),1.79(1H,d,J=14.0Hz,H-12α),1.61(1H,brd,H-10β),1.46(1H,dt,J=11.0,2.5Hz,H-10α),1.25(1H,m,H-9α),1.11(3H,s,H-14),1.19(3H,s,H-15),0.88(3H,d,J=7.0Hz);13C-NMR(125MHz,CDCl3)δC:162.7(C-5),104.3(C-6),77.3(C-4),58.5(C-1),55.6(C-12),49.3(C-11),46.1(C-2),39.1(C-13),39.0(C-3),38.3(C-8),35.1(C-15),28.2(C-10),26.9(C-14),26.3(C-9),17.6(C-7)。; 上述NMR数据与文献[4]报道一致,确证该化合物为suberosenolA。化合物2白色粉末,mp142~144℃,ESI-MSm/z221[M+H]+。1H-NMR(500MHz,CDCl3)δH:5.17(1H,s,H-6a),4.79(1H,s,H-6b),4.56(1H,d,5.5,H-4),2.39(1H,dd,J=11.5,7.5Hz,H-2),1.78(1H,ddd,J=13.5,7.5,4.0Hz,H-3α),2.08(1H,ddd,J=13.5Hz,7.0Hz,4.5Hz,H-3β),2.01(2H,m,H-8,9β),1.77(1H,m,H-11),1.66(1H,d,J=14.0Hz,H-12α),1.60(1H,m,H-10β),1.57(1H,d,J=14.0Hz,H-12β),1.48(1H,m,H-10α),1.28(1H,m,H-9α),1.15(3H,s,H-15),1.10(3H,s,H-14),0.96(3H,d,J=7.0Hz,H-7);13C-NMR(125MHz,CDCl3)δC:162.2(C-5),107.6(C-6),76.7(C-4),59.0(C-1),55.0(C-12),49.7(C-11),49.0(C-2),39.7(C-13),37.8(C-3),36.9(C-8),34.9(C-15),27.9(C-10),26.9(C-14),26.7(C-9),17.8(C-7)。; 上述NMR数据与文献[4]报道一致,确证该化合物为suberosenolB。化合物3无色油状物,mp252~254℃,ESI-MSm/z219[M+H]+。1H-NMR(500MHz,CDCl3)δH:5.97(1H,d,J=0.75Hz,H-6a),4.98(1H,d,J=0.75Hz,H-6b),2.67(1H,dd,J=19.0,11.5Hz,H-3β),2.45(1H,dd,J=19.0,9.5Hz,H-3α),2.33(1H,t,J=11.5Hz,H-2),2.15(2H,m,H-8),2.08(1H,m,H-9β),1.88(1H,brs,H-11),1.80(1H,d,J=14.5Hz,H-12a),1.70(1H,d,J=14.5Hz,H-12b),1.71(1H,m,H-10β),1.60(1H,m,H-10α),1.35(1H,ddd,J=13.0,5.5,1.0Hz,H-9α),1.20(3H,s,H-15),1.17(3H,s,H-14),0.90(3H,d,J=7.0Hz,H-7);13C-NMR(125MHz,CDCl3)δC:208.5(C-4),151.8(C-5),115.3(C-6),57.8(C-1),54.3(C-12),49.