详细信息
New chromatographic stationary phase, which is hydrophilic and highly selective, and has high conversion rate
文献类型:专利
英文题名:New chromatographic stationary phase, which is hydrophilic and highly selective, and has high conversion rate
作者:CHU C;GUO R;YIN W;CHENG Z;LI Y;ZHU Z
机构:[1]UNIV EAST CHINA SCI & TECHNOLOGY
申请号:CN104826618-B
公开日:2017-05-24
语种:英文
收录:DERWENT
摘要:NOVELTY - Chromatographic stationary phase (I) is new. USE - Chromatographic stationary phase. ADVANTAGE - The chromatographic stationary phase is hydrophilic and highly selective, and has high conversion rate. DETAILED DESCRIPTION - Chromatographic stationary phase of formula (I) is new. An INDEPENDENT CLAIM is included for a method for preparing chromatographic stationary phase, which involves: (A) mixing silane coupling agent (III) and 2-propynylamine with organic solvent at 60-150 degrees C for 6-36 hours, where silane coupling agent and 2-propynylamine are mixed in ratio of 1-5:1.2-5; (B) adding 1-10mmol activated silica gel microsphere to the obtained mixture at 80-120 degrees C for 12-48 hours; (C) filtering the obtained mixture through funnel; (D) washing the obtained precipitate with dichloromethane, methanol and acetone to obtain solid; (E) drying the obtained solid under vacuum at 40-80 degrees C for 6-12 hours to obtain silica with terminal alkynyl group; (F) preparing terminal alkynyl by mixing silica in mixture containing water and methanol in ratio of 2-10:1; (G) mixing obtained mixture with mixture containing water and methanol (20-50ml) to obtain silica alkynyl (II); (H) modifying silica alkynyl by mixing with azide group having aminodiol structure (IV) (1-15 times of the amount of silica alkynyl) and catalyst, where catalyst is copper sulfate (1-10%) and sodium ascorbate(2-40%); (I) incubating the obtained reaction mixture at 10-80 degrees C for 72-100 hours; (J) filtering the obtained reaction mixture; (K) washing the obtained precipitate with water; (L) adding 2-20 wt.% EDTA disodium solution; (M) washing the obtained material with water, methanol and acetone to obtain solid matter; and (N) vacuum-drying the obtained solid at 40-80 degrees C for 6-12 hours to obtain chromatographic stationary phase. .
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