With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.88150-62-3, name is Phthaloylamlodipine, molecular formula is C28H27ClN2O7, molecular weight is 538.98, as common compound, the synthetic route is as follows.Computed Properties of C28H27ClN2O7
Example (1)100 g (0.185 mol) of phthaloyl amlodipine and toluene (1-1.5 L) were charged to 2 L autoclave. Methylamine gas was purged to the above reaction mass at room temperature. The reaction mass was stirred at 40-70 C for 8-10 hrs. and then at room temperature (25 C) for 8-12 hrs to complete the reaction. The completion of the reaction was monitored by TLC. After completion of the reaction, IPA (400 mL) was added to the reaction mixture and further stirred for 10-20 min. The reaction mixture was washed with 2 x 400 mL of water. The organic layer was separated and the volume was reduced to 100-150 mL by evaporation under vacuum. Hexane (1-1.5 L) was added slowly (20-30 min) to the above concentrated mass at 40-50 C. The solid obtained was filtered and dried at 45-50 C for 10-15 hrs. to obtain 55-70 g of amlodipine free base as the product.Example (2)100 g (0.185 mol) of phthaloyl amlodipine and isopropyl alcohol (1L) were charged to a 2 L autoclave. Methylamine gas was purged to the above reaction mass at room temperature. The reaction mass was stirred at 50 C for 4-8 hrs. and then at room temperature for 8-12 hrs for the reaction to complete. The completion of the reaction was monitored by TLC. The reaction mass was filtered and the filtrate was concentrated to syrupy mass at reduced pressure and at bath temperature of about 40- 50 C. To the above residue toluene (600 mL) was added and was stirred for 20-40 min. The reaction mixture was washed with 3 x 300 mL of water. The organic layer was separated, dried over sodium sulfate and was evaporated under vacuum to near completion by maintaining the bath temperature at 50-60 C. Hexane (1-1.5 L) was added slowly (20-30 min) to the above concentrated mass at 40-50 C. The solid obtained was filtered and dried at 45-50 C for 10-15 hours to obtain 55-70 g of amlodipine free base as the product.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,88150-62-3, Phthaloylamlodipine, and friends who are interested can also refer to it.
Reference:
Patent; ORCHID CHEMICALS & PHARMACEUTICALS LIMITED; WO2007/96724; (2007); A1;,
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