本文报道了从三尖杉碱合成三尖杉酯碱的工作,以γ-甲基1,4-戊内酯(Ⅰ)作原料,得到关键中间体5,5-二甲基2-羟基四氢呋喃-2(Ⅴ),(Ⅴ)易脱水得5,5-二甲基二氢呋喃酸-2(Ⅵ),用(Ⅵ)的钠盐(Ⅶ)制备酰氯(Ⅷ),然后在无水吡啶中与三尖杉碱反应得相应的酯(Ⅸ),(Ⅸ)用盐酸、醋酸处理加水得(Ⅹ),通过Reformatsky反应得到最终产物三尖杉酯碱及其差向异构体的混合物(ⅪⅤ),可用反流分布法或中性氧化铝干柱层析法提纯,经薄层定量测定,三尖杉酯碱及表三尖杉酯碱的相对合量粗略相等。 This paper reports the synthesis of harringtonine from cephaloxine, using γ-methyl 1,4-valerolactone (Ⅰ) as the raw material to obtain the key intermediate of 5,5-dimethyl 2-hydroxytetrahydrofuran (V) is easily dehydrated to give 5,5-dimethyldihydrofuran-2 (Ⅵ). The acid chloride (Ⅷ) is prepared from the sodium salt of (Ⅵ) (VII) (Ⅸ), (IX) is treated with hydrochloric acid, acetic acid and water is added (X) to obtain the final product harringtonine and its epimer by a Reformatsky reaction XIV), which can be purified by reflux distribution method or neutral alumina dry column chromatography. The relative amounts of harringtonine and harringtonine are approximately the same by TLC.