Method for preparing R-lipoic acid choline ester halide
A lipoic acid choline and halide technology, which is applied in the field of pharmaceutical chemical synthesis, can solve the problems of unspecified preparation conditions and operations, and achieve the effects of safe use, reasonable technical solutions, and simplified operations
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Embodiment 1
[0027] Method A): Add R-lipoic acid (10.0g, 48.5mmol) and toluene (200mL) into a reaction flask, stir to dissolve, add N,N'-dicyclohexylcarbodiimide (12.0g, 58.2mmol) and 4-Dimethylaminopyridine (1.2g, 9.7mmol) was cooled in an ice bath, choline chloride (15.2g, 109.1mmol) was added, and the reaction mixture was reacted at 35°C for 18h. Post-treatment and purification, the crude product was recrystallized with isopropanol to obtain R-lipoic acid choline ester chloride, a light yellow solid (14.8g), with a yield of 93%, and the reaction formula was:
[0028]
Embodiment 2
[0030] Method B): Add R-lipoyl chloride (10.0g, 44.5mmol) and chloroform (200mL) into a reaction flask, stir to dissolve, add N,N-diethylaniline (26.6g, 178.0mmol), cool in an ice bath, Choline chloride (18.6g, 133.5mmol) was added, and the reaction mixture was reacted at 20°C for 12h. Post-treatment and purification, the crude product was recrystallized with isopropanol to obtain R-lipoic acid choline ester chloride, a light yellow solid (12.7g), with a yield of 87%, and the reaction formula was:
[0031]
Embodiment 3
[0033] Method A): Add R-lipoic acid (10.0g, 48.5mmol) and 1,2-dichloroethane (200mL) into the reaction flask, stir to dissolve, add N,N'-carbonyldiimidazole (8.6g, 53.3mmol ) and 2,6-lutidine (0.5g, 4.8mmol), cooled in an ice bath, added choline bromide (26.8g, 145.4mmol), and the reaction mixture was reacted at 20°C for 24h. Post-treatment and purification, the crude product was recrystallized with isopropanol to obtain R-lipoic acid choline ester bromide as a light yellow solid (17.1g), with a yield of 95%. The reaction formula is:
[0034]
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