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    • 6. 发明申请
    • YIELD-EFFICIENT PROCESS FOR THE PRODUCTION OF HIGHLY PURE 2-METHYL-1,4-NAPHTHOQUINONE AND ITS DERIVATIVES
    • 用于生产高纯度2-甲基-1,4-萘醌及其衍生物的有效方法
    • WO2011085945A1
    • 2011-07-21
    • PCT/EP2011/000024
    • 2011-01-06
    • LONZA LTDAMOUZEGAR, KamyabMAHDAVI, BehzadLANGEVIN, MathieuDIDIER, CharlesLIEB, Alexander
    • AMOUZEGAR, KamyabMAHDAVI, BehzadLANGEVIN, MathieuDIDIER, CharlesLIEB, Alexander
    • C07C46/04
    • C07C46/04C07C46/08C07C50/12
    • The present invention discloses a process for the production of 2-methyl-1,4-naphthoquinone and its bisulfite adducts, comprising the following steps: a) oxidizing 2-methyl-naphthalene (2-MNA) to achieve an organic phase containing 2-methyl-naphthoquinone (2-MNQ) and 6-methyl-naphthoquinone (6-MNQ); b) subjecting said organic phase to treatment with an aqueous solution of a bisulfite salt to extract preferentially the 6-MNQ isomer from the organic phase; c) separating said organic phase from the aqueous phase; d) subjecting the organic phase of process step c) to a second bisulfitation step with an aqueous solution of a bisulfite salt, resulting in an organic phase containing 2-MNA and trace amounts of 2-MNQ and an aqueous phase containing 2-MSB and trace amounts of 6-MSB; e) optionally removing interfering bisulfite ions from the aqueous phase of process step c); f) raising the pH of the aqueous phase from step c) or e) to higher than 8,5 in the presence of a solvent resulting in an organic phase containing 2-MNQ; g) combining the organic phase from step f) with the organic phase being treated in the process step d); h) recycling the organic phase from step d) back to step a) to be used as solvent for the oxidation reaction of 2-MNA.
    • 本发明公开了一种2-甲基-1,4-萘醌及其亚硫酸氢盐加合物的制备方法,包括以下步骤:a)氧化2-甲基 - 萘(2-MNA)以获得含2- 甲基萘醌(2-MNQ)和6-甲基萘醌(6-MNQ); b)使用亚硫酸氢盐水溶液对所述有机相进行处理,从有机相中优先提取6-MNQ异构体; c)将所述有机相与水相分离; d)使工艺步骤c)的有机相与亚硫酸氢盐水溶液进行第二次双硫化步骤,得到含有2-MNA和痕量2-MNQ的有机相和含有2-MSB的水相和 痕量6-MSB; e)任选地从工艺步骤c)的水相中除去干扰亚硫酸氢盐离子; f)在溶剂存在下将水相的pH从步骤c)或e)提高到高于8.5,导致含有2-MNQ的有机相; g)将步骤f)中的有机相与方法步骤d)中待处理的有机相结合; h)将步骤d)中的有机相回收至步骤a)以用作2-MNA的氧化反应的溶剂。