资源描述:
《-甲基吡啶 丁炔二酸二甲酯 -氯靛红(溴化苄) 对甲基苯乙酮 - wiley》由会员上传分享,免费在线阅读,更多相关内容在教育资源-天天文库。
1、Athree-componentreactionfortheefficientconstructionofthe2',11b'-dihydrospiro[indoline-3,1'-pyrido[2,1-a]isoquinoline]skeletonJingSun,YanSun,HuiGong,Chao-GuoYan*SupportingInformationGeneralExperimentalMethodsandCharacterizationofcompounds2-24X-RayCrystallographicData:CIFinseparatefile.Crystallo
2、graphicdata1c(CCDC 916459),2b(CCDC 915460)and3b(CCDC 915461)havebeendepositedvattheCambridgeCrystallographicDatabaseCentreandisavailableonrequestfromtheDirector,CCDC,12UnionRoad,Cambridge,CB21EZ,UK(http//www.ccdc.cam.ac.uk).24dimethyl1-benzyl-5-fluoro-2'-(4-methoxybenzoyl)-2-oxo-2',11b'-dihydr
3、ospiro[indoline-3,1'-pyrido[2,1-a]isoquinoline]-3',4'-dicarboxylate(1a):yellowsolid,35%,m.p.187~189℃;1HNMR(600MHz,DMSO-d6)δ:7.76(d,J=8.4Hz,2H,ArH),7.25(brs,3H,ArH),7.08~7.04(m,4H,ArH),6.92(d,J=7.2Hz,1H,ArH),6.88(d,J=8.4Hz,2H,ArH),6.79~6.77(m,1H,ArH),6.75(d,J=8.4Hz,1H,ArH),6.57(t,J=7.8Hz,1H,ArH
4、),6.48(d,J=7.8Hz,1H,ArH),6.21(d,J=7.8Hz,1H,CH),5.83(d,J=7.8Hz,1H,CH),5.72(s,1H,CH),5.03(d,J=15.6Hz,1H,CH),4.78(s,1H,CH),4.67(d,J=15.6Hz,1H,CH),3.87(s,3H,OCH3),3.79(s,3H,OCH3),3.44(s,3H,OCH3);13CNMR(150MHz,DMSO-d6)δ:198.0,137.7,165.4,164.5,163.3,157.3(d,J=236.3Hz),145.2,138.8,135.7,131.5,130.9,
5、130.2,129.0,128.5,128.2,127.4,127.2,126.7,125.6,125.5,124.6,115.2(d,J=23.7Hz),114.0(d,J=26.6Hz),110.5(d,J=7.4Hz),106.4,102.2,57.3,55.5,53.1,51.6,49.7,43.7,43.1;IR(KBr)υ:3450,1737,1706,1662,1601,1571,1493,1453,1425,1383,1358,1313,1285,1262,1231,1211,1178,1138,1111,1058,1026,973,930,853,813,773c
6、m-1;MS(m/z):HRMS(ESI)Calcd.forC39H32FN2O7([M+H]+):659.2188.Found:659.2188.24dimethyl1-benzyl-5-fluoro-2'-(4-methoxybenzoyl)-2-oxo-2',11b'-dihydrospiro[indoline-3,1'-pyrido[2,1-a]isoquinoline]-3',4'-dicarboxylate(2a):yellowsolid,45%,m.p.191~193℃;1HNMR(600MHz,DMSO-d6)δ:7.60(d,J=8.4Hz,2H,ArH),7.1
7、3(t,J=7.8Hz,1H,ArH),7.09(t,J=7.2Hz,2H,ArH),7.00~7.63(m,6H,ArH),6.86~6.82(m,1H,ArH),6.78(d,J=7.8Hz,1H,ArH),6.53~6.50(m,3H,ArH,CH),6.24(dd,J1=8.6Hz,J2=4.3Hz,1H,ArH),5.59(s,1H,CH),5.42(s,1H,CH),5.39(d,J=7.8Hz,1H,CH),4.59(d,J=15.9Hz,1H,CH),