A kind of synthetic method of -2-(2,5-difluorophenyl) pyrrolidine hydrochloride
A technology of pyrrolidine hydrochloride and difluorophenyl, which is applied in the field of drug synthesis, can solve the problems of difficulty in obtaining and harsh reaction conditions, and achieves the effects of high safety, mild reaction conditions, and increased safety and operability.
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Embodiment 1
[0023] Synthesis of Intermediate I
[0024] Dichloromethane (300 mL) was added to a 2 L three-necked flask, and aluminum trichloride (283.4 g, 2.5 mol) and succinic anhydride (120.1 g, 1.2 mol) were added in sequence under stirring, and the temperature was raised to 35 °C. Fluorobenzene (114.1 g, 1 mol) was added dropwise to the reaction system, the dropwise addition was completed in 0.5 h, and the reaction was maintained at 35-38 °C for 4 h. TLC monitored the completion of the reaction. Then the reaction solution was slowly poured into ice water (500 g), then concentrated hydrochloric acid (0.9 L, 6 M) solution was added, stirred for 0.5 h, the organic phase was separated, and the aqueous phase was extracted once with dichloromethane (100 mL), The organic phases were combined, washed once with water (300 mL), dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a crude product, which was recrystallized from toluene to obtain 183.1 g of a whit...
Embodiment 2
[0032] Synthesis of Intermediate I
[0033] Dichloromethane (600 mL) was added to a 5 L three-necked flask, and aluminum trichloride (566.8 g, 5.0 mol) and succinic anhydride (240.2 g, 2.4 mol) were added in sequence under stirring, and the temperature was raised to 35 °C. Fluorobenzene (228.2 g, 2 mol) was added dropwise to the reaction system, the dropwise addition was completed in 0.5 h, and the reaction was maintained at 35-38 °C for 4 h. TLC monitored the completion of the reaction. Then the reaction solution was slowly poured into ice water (1000 g), then concentrated hydrochloric acid (1.8 L, 6 M) solution was added, stirred for 0.5 h, the organic phase was separated, and the aqueous phase was extracted once with dichloromethane (200 mL), The organic phases were combined, washed once with water (600 mL), dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a crude product, which was recrystallized from toluene to obtain 382.1 g of a whi...
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