化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2014年
9期
1441-1444
,共4页
L-组氨酸%选择性%不对称合成
L-組氨痠%選擇性%不對稱閤成
L-조안산%선택성%불대칭합성
L-histidine%selectivity%asymmetric synthesis
研究了异丁醛与乙醛酸乙酯不对称羟醛缩合反应合成(R)-3,3-二甲基-2-羟基-4-氧代丁酸乙酯,考察了催化剂种类及用量、反应时间、反应溶剂对羟醛缩合反应的影响。确定较佳反应条件为：L-组氨酸作催化剂,用量为乙醛酸乙酯物质的量的30%,乙二醇为溶剂,反应时间24h。( R)-3,3-二甲基-2-羟基-4-氧代丁酸乙酯的收率达75%,ee值为73%。产物结构经1 H NMR,GC-MS进行了表征。
研究瞭異丁醛與乙醛痠乙酯不對稱羥醛縮閤反應閤成(R)-3,3-二甲基-2-羥基-4-氧代丁痠乙酯,攷察瞭催化劑種類及用量、反應時間、反應溶劑對羥醛縮閤反應的影響。確定較佳反應條件為：L-組氨痠作催化劑,用量為乙醛痠乙酯物質的量的30%,乙二醇為溶劑,反應時間24h。( R)-3,3-二甲基-2-羥基-4-氧代丁痠乙酯的收率達75%,ee值為73%。產物結構經1 H NMR,GC-MS進行瞭錶徵。
연구료이정철여을철산을지불대칭간철축합반응합성(R)-3,3-이갑기-2-간기-4-양대정산을지,고찰료최화제충류급용량、반응시간、반응용제대간철축합반응적영향。학정교가반응조건위：L-조안산작최화제,용량위을철산을지물질적량적30%,을이순위용제,반응시간24h。( R)-3,3-이갑기-2-간기-4-양대정산을지적수솔체75%,ee치위73%。산물결구경1 H NMR,GC-MS진행료표정。
Ethyl(R)-3,3-dimethyl-2-hydroxy-4-oxobutyrate was synthesized by asymmetric aldol reaction using ethyl glyoxylate and isobutyraldehyde as raw material. The effects of aldol reaction conditions,including the type and amount of catalyst,reaction time, reaction solvent,were investigated. The optimal conditions were as follows:L-histidine as catalyst at an amount of 30%of the molar ratio of ethyl glyoxylate. The yield of(R)-3,3-dimethyl-2-hydroxy-4-oxobutyric acid ethyl ester reached 75%in which the enantions-electivity( e. e) of the product gained 73%. The product was characterized by 1 H NMR and GC-MS.
