A kind of synthetic method of vildagliptin intermediate
A synthesis process and pyrrolidine technology, applied in organic chemistry and other directions, can solve the problems of complicated operation, high price, high reaction cost, separation and purification, etc., and achieve the effect of reducing workload, easy operation, and avoiding production of by-products
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Embodiment 1
[0014] Add 20.0g L-proline to the 250ml reaction bottle, and then add 100ml tetrahydrofuran. While stirring, 30ml of chloroacetyl chloride was added dropwise. After the dropwise addition was completed, the mixture was stirred at room temperature for 4 h. Reactions were monitored with TLC plates. After the reaction is complete, add 40 ml of distilled water and continue to stir for 20 min. After stirring, 100ml of ethyl acetate and 60ml of distilled water were added to the reaction solution. Then pour into a separatory funnel, let it stand, and collect the organic layer. The aqueous layer was extracted twice with 200 ml ethyl acetate. The organic layers were combined and dried by adding anhydrous sodium sulfate for 20 h. After drying, the organic solvent was evaporated by rotary evaporation. Add 320ml of tetrahydrofuran, 48g of di-tert-butyl dicarbonate, and 128g of ammonium bicarbonate to 28g of oil, and stir. When a white turbid solution appears, add 8ml of pyridine, and ...
Embodiment 2
[0016] Add 40.0gL-proline to the 500ml reaction bottle, and then add 200ml tetrahydrofuran. While stirring, 60ml of chloroacetyl chloride was added dropwise. After the dropwise addition was completed, the mixture was stirred at room temperature for 4 h. Reactions were monitored with TLC plates. After the reaction is complete, add 40 ml of distilled water and continue to stir for 20 min. After stirring, 200ml of ethyl acetate and 120ml of distilled water were added to the reaction solution. Then pour into a separatory funnel, let it stand, and collect the organic layer. The aqueous layer was extracted twice with 400 ml ethyl acetate. The organic layers were combined and dried by adding anhydrous sodium sulfate for 20 h. After drying, the organic solvent was evaporated, and the oil weighed 55g. Add 640ml of tetrahydrofuran, 96g of di-tert-butyl dicarbonate, and 256g of ammonium bicarbonate, and stir. When a white turbid solution appeared, add 16ml of pyridine, and then stir...
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