{"title":"利用n -膦基官能团保护氨基酸的基团辅助纯化(GAP)(在Kuwajima教授77岁生日之际献给他)","authors":"Guanghui An, Cole Seifert, Hao Sun","doi":"10.3987/COM-14-S(K)25","DOIUrl":null,"url":null,"abstract":"General The 1 H NMR, 13 C NMR and 31 P NMR spectra were recorded on a Jeol eclipse 400 SS (operating at 400 MHz for proton) at ambient temperature. The ESI-MS and ESI-HRMS were recorded with an Exactive (Thermo Scientific, San Jose, CA) mass spectrometer. Dry dichloromethane (DCM) was bought from Acros Organics and used directly. N, N’dimethylformamide (DMF) was dried over 4 Å molecule sieves powder. 4Ǻ molecular sieves powder was activated by heating in oven at 120 o C for 24 hours. Triethylamine was stand over KOH solid overnight and distilled before use. Tetrahedron furan (THF) was distilled from Na metal before use. All the other chemicals were bought from commercial source and used directly after arrival.","PeriodicalId":12850,"journal":{"name":"Heterocycles : an international journal for reviews and communications in heterocyclic chemistry","volume":"130 1","pages":"344-356"},"PeriodicalIF":0.0000,"publicationDate":"2015-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"3","resultStr":"{\"title\":\"GROUP-ASSISTED PURIFICATION (GAP) FOR PROTECTION OF AMINO ACIDS USING N-PHOSPHONYL FUNCTIONAL GROUPS (Dedicated to Professor Isao Kuwajima on the occasion of his 77th birthday)\",\"authors\":\"Guanghui An, Cole Seifert, Hao Sun\",\"doi\":\"10.3987/COM-14-S(K)25\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"General The 1 H NMR, 13 C NMR and 31 P NMR spectra were recorded on a Jeol eclipse 400 SS (operating at 400 MHz for proton) at ambient temperature. The ESI-MS and ESI-HRMS were recorded with an Exactive (Thermo Scientific, San Jose, CA) mass spectrometer. Dry dichloromethane (DCM) was bought from Acros Organics and used directly. N, N’dimethylformamide (DMF) was dried over 4 Å molecule sieves powder. 4Ǻ molecular sieves powder was activated by heating in oven at 120 o C for 24 hours. Triethylamine was stand over KOH solid overnight and distilled before use. Tetrahedron furan (THF) was distilled from Na metal before use. All the other chemicals were bought from commercial source and used directly after arrival.\",\"PeriodicalId\":12850,\"journal\":{\"name\":\"Heterocycles : an international journal for reviews and communications in heterocyclic chemistry\",\"volume\":\"130 1\",\"pages\":\"344-356\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2015-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"3\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Heterocycles : an international journal for reviews and communications in heterocyclic chemistry\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.3987/COM-14-S(K)25\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Heterocycles : an international journal for reviews and communications in heterocyclic chemistry","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.3987/COM-14-S(K)25","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 3
摘要
1 H NMR, 13 C NMR和31 P NMR光谱记录在Jeol月食400 SS(质子工作在400 MHz)在环境温度下。ESI-MS和ESI-HRMS用Exactive (Thermo Scientific, San Jose, CA)质谱仪记录。干二氯甲烷(DCM)从Acros Organics购买并直接使用。N, N '二甲基甲酰胺(DMF)在4个Å分子筛上干燥成粉末。4Ǻ分子筛粉经120℃烤箱加热24小时活化。三乙胺放置在KOH固体上过夜并在使用前进行蒸馏。使用前从Na金属中蒸馏出四面体呋喃(THF)。所有其他化学品都是从商业来源购买的,并在抵达后直接使用。
GROUP-ASSISTED PURIFICATION (GAP) FOR PROTECTION OF AMINO ACIDS USING N-PHOSPHONYL FUNCTIONAL GROUPS (Dedicated to Professor Isao Kuwajima on the occasion of his 77th birthday)
General The 1 H NMR, 13 C NMR and 31 P NMR spectra were recorded on a Jeol eclipse 400 SS (operating at 400 MHz for proton) at ambient temperature. The ESI-MS and ESI-HRMS were recorded with an Exactive (Thermo Scientific, San Jose, CA) mass spectrometer. Dry dichloromethane (DCM) was bought from Acros Organics and used directly. N, N’dimethylformamide (DMF) was dried over 4 Å molecule sieves powder. 4Ǻ molecular sieves powder was activated by heating in oven at 120 o C for 24 hours. Triethylamine was stand over KOH solid overnight and distilled before use. Tetrahedron furan (THF) was distilled from Na metal before use. All the other chemicals were bought from commercial source and used directly after arrival.