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在Stork烯胺酰化反应中,通常需添加一个三级胺以中和反应中生成的氯化氢。产物常是液体或低熔点固体,不易提纯、析离。本文使用N-甲基哌嗪代替吗啉等常用的环状仲胺,考察其中的三级胺基能否起到外加三级胺的作用,并使酰化产物(Ⅲ)形成便于离析的盐酸盐结晶。我们以N-甲基哌嗪的环戊酮和环己酮烯胺为代表进行了乙酰化和苯甲酰化,析离了单酰基化产物Ⅲ(a1),Ⅲ_(a2)和Ⅲ_(b1)及其相应的水解产物Ⅳ_(a1),Ⅳ_(a2),Ⅳ_(b1)和Ⅳ_(b2);还得到了三个二酰基化产物。
In the Stork enamoylation reaction, it is usually necessary to add a tertiary amine to neutralize the hydrogen chloride formed in the reaction. Products are often liquid or low melting point solid, not easy to purify, separation. In this paper, N-methylpiperazine was used instead of the commonly used cyclic secondary amines such as morpholine to investigate whether the tertiary amine group could act as an additional tertiary amine and to make the acylated product (III) form a salt for segregation Acid salt crystallization. We acetylated and benzoylated with cyclopentanone and cyclohexanone enamine of N-methylpiperazine, separated the monoacylated products Ⅲ (a1), Ⅲ_ (a2) and Ⅲ_ (b1 ) And its corresponding hydrolysates Ⅳ_ (a1), Ⅳ_ (a2), Ⅳ_ (b1) and Ⅳ_ (b2). Three diacylated products were also obtained.