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作为合成SB_1的中间体γ-氯代-γ-乙酰基丙醇乙酯,在制备上有不少问题,主要是氯化一步,有多氯化合物生成,故须经严格分离,否则用于SB_1合成,对产率影响很大。鉴于上述情况,试验了以丁炔二醇为起始原料合成α-氯-α-乙酰-γ-丁內酯的路线: 丁炔二醇合成是参照Reppe法,以硅石为载体的乙炔铜催化剂,在塔式反应器中进行连续常压反应,甲醛总转化率可达80％左右,收率75—80％,触媒可连续使用1000—1500小时。丁炔二醇以活性镍和醋酸酮混合催化剂控制pH8.5进行加氢反应,丁二醇收率可达
As an intermediate in the synthesis of SB_1, γ-chloro-γ-acetyl-propanol ethyl ester, there are many problems in the preparation, mainly chlorinated one step, the formation of polychlorinated compounds, it must be strictly separated, otherwise used for SB_1 Synthesis, a great impact on the yield. In view of the above, we have tested the route of synthesizing α-chloro-α-acetyl-γ-butyrolactone from butynediol as the starting material: the reaction of butynediol with reference to Reppe method, silica supported acetylene copper catalyst , Continuous atmospheric reaction in a tower reactor, the total conversion of formaldehyde up to 80%, the yield of 75-80%, the catalyst can be used continuously for 1000-1500 hours. Butynediol with active nickel and acetic acid ketone mixed catalyst control pH8.5 hydrogenation reaction, butanediol yield up