Preparation method of Elagolix intermediate 2-fluoro-6-trifluoromethyl benzylamine
A technology of trifluoromethylbenzylamine and trifluoromethyl, applied in the preparation field of Elagolix intermediate 2-fluoro-6-trifluoromethylbenzylamine, can solve the problem of 2-fluoro-6-trifluoromethylbenzylamine The problems of expensive raw materials for amine synthesis, to achieve the effect of cheap raw materials, conducive to industrial production, and high purity
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[0029] (1) 2-Fluoro-6-(trifluoromethyl)benzoic acid (e.g. figure 2 )Synthesis.
[0030] In a 2L four-neck flask equipped with a thermometer, mechanical stirring, and constant pressure dropping funnel device, add 50g (0.3mol) of 3-fluorobenzotrifluoride and 500ml of anhydrous tetrahydrofuran under nitrogen protection, and cool the liquid nitrogen to -78℃. Add 190.5ml (1.6M) of n-butyllithium dropwise, the temperature is controlled at -60~-65℃, after the addition is completed, the temperature is controlled at -60~-65℃, continue to stir for 5 hours, and pass carbon dioxide gas until The reaction was completed; a small amount of water was added to quench the reaction, and the reaction was raised to room temperature; hydrochloric acid was adjusted to pH 2, 500 ml of ethyl acetate was added, and the organic layer was separated; the organic layer was concentrated under reduced pressure to obtain 53 g of white solid, yield 85%, purity 98 %.
[0031] (2) 2-Fluoro-6-(trifluoromethyl)benzyl...
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