Bis(trifluoroethyl) methylphosphonate is the starting material for the synthesis of Jin’s reagent. Jin’s reagent is widely used for the preparation of (Z)-α,β-unsaturated ketones and is also a valuable potent flame-retardant additive. Preparation of bis(trifluoroethyl) methylphosphonate was investigated by direct transesterification of dimethyl methylphosphonate with 2,2,2-trifluoroethanol (further trifluoroethanol, TFE), being a well-known weak nucleophile, using microwave and flow reactors. Direct transesterification was successful in a continuous flow reactor at 450 °C and 200 bar using a highly diluted reaction mixture. The product, bis(trifluoroethyl) methylphosphonate, was purified by column chromatography, and excess trifluoroethanol was recovered by distillation.

中文翻译：

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制备双（2,2,2-三氟乙基）甲基膦酸酯的绿色工艺

双（三氟乙基）甲基膦酸酯是合成金氏试剂的起始原料。Jin的试剂被广泛用于制备（Z）-α，β-不饱和酮，也是一种有价值的强效阻燃添加剂。通过使用微波和流动反应器，通过将甲基膦酸二甲酯与众所周知的弱亲核试剂2,2,2-三氟乙醇（进一步的三氟乙醇，TFE）直接酯交换，研究了甲基二膦酸三（三氟乙基）酯的制备。使用高度稀释的反应混合物，在450°C和200 bar的连续流反应器中成功进行了直接酯交换反应。通过柱色谱法纯化产物双（三氟乙基）甲基膦酸酯，并通过蒸馏回收过量的三氟乙醇。