摘要
在过量的亚磷酸三丁酯（２）及活性锌存在下，２＇－氧－６＇－甲基－庚酰三尖杉碱（１）与α－溴代乙酸甲酯不发生Ｒｅｆｏｒｍａｔｓｋｙ反应，而由１与２反应得到一种新的含磷三尖杉酯碱－２＇－羟基－２＇－［二正丁氧基］－膦酰基－６＇－甲基－庚酰三尖杉碱（３）及其差向异构体（３＇）及其差向异构体（３＇）的混合物。两者比例为７５：２５％，经硅胶薄层层离或柱层析分离得到纯品。它们的结构由ＩＲ。
In the presence of freshly prepared active zinc and excess tributyl phosphite(2),2′-oxo-6′-methyl heptanoyl cephalotaxine(1)and methyl bromoacetate,Refor-matsky reaction did not take place,but afforded a mixture of 2′-hydroxy-2′[-di-n-bu-toxyl]-phosphonyl-6′-methyl -heptanoyl-cephalotaxine(3)and its epimer(3′)with a ra-tio of 75:25.The separation of 3 and 3'was achieved by means of silica gel tic plate andcolumn chromatography when a mixture of CHCl_3-CH_3OH(9:1v/v)was used as devel-oping solvent.The assignment of structures of 3 and 3'was done by comparing their IR,H-NMR and MS spectra with those of homodeoxyharringtonine(4)and epihomodeoxy-harringtonine(4′)
出处
《兰州大学学报（自然科学版）》
CAS
CSCD
北大核心
1993年第4期127-131,共5页
Journal of Lanzhou University(Natural Sciences)
基金
国家自然科学基金
关键词
三尖杉碱
合成
氮杂环化合物
cephalotaxine
synthesis
nitrogen hetero cyclics
Reformatsky reaction
phosphorus-bearing cephalotaxus ester alkaloid
