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A Green Process for the Preparation of Bis(2,2,2-trifluoroethyl) Methylphosphonate
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2017-12-05 00:00:00 , DOI: 10.1021/acs.oprd.7b00274
Katalin Molnár 1 , László Takács 1 , Ferenc Faigl 2 , Zsuzsanna Kardos 1
Affiliation  

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:

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。
更新日期:2017-12-05
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