Method for synthesizing trifluoromethyl amine
The technology of a trifluoromethyl-substituted amine and a synthetic method, which is applied in the field of preparation of trifluoromethyl-containing compounds, can solve the problems of cumbersome steps, high yield, expensive fluorocarbon nitrile, etc., and achieve short process flow and high yield , the effect of easy product
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Embodiment 1
[0029] Put 1 mole of D-alanine and 12 moles of anhydrous hydrofluoric acid into a 1L stainless steel (316L material) autoclave, stir for 15 minutes, add 2.2 moles of sulfur tetrafluoride, and react at 85°C for 4 hours. After the reaction, the temperature was lowered to room temperature, the by-product thionyl fluoride and unreacted sulfur tetrafluoride were absorbed with lye, the reaction solution was poured into ice water, neutralized to alkaline with sodium hydroxide, and then extracted with dichloromethane. The extract was separated by distillation to obtain 0.86 moles of the product (S)-trifluoroisopropylamine, with a content of 99%, and a yield of 86% based on D-alanine.
Embodiment 2
[0031] The reaction device and operation steps are the same as those in Example 1, except that 1 mole of D-alanine, 3 moles of anhydrous hydrofluoric acid, and 3.2 moles of sulfur tetrafluoride are added, and the reaction is carried out at 85° C. for 3.5 hours. 0.65 mol of (S)-trifluoroisopropylamine was obtained, with a content of 97.8%, and a yield of 65% based on D-alanine.
Embodiment 3
[0033] The reaction device and operation steps are the same as those in Example 1, except that 1 mole of D-alanine, 20 moles of anhydrous hydrofluoric acid, and 1.8 moles of sulfur tetrafluoride are added, and the reaction is carried out at 85° C. for 10 h. 0.76 moles of (S)-trifluoroisopropylamine were obtained, with a content of 98.8%, and a yield of 76% based on D-alanine.
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