反应详情

Citalopram base (167 g) was dissolved in acetone (837 ml). Thereto was blown in a hydrobromic acid gas at 15° C.-40° C. to make the pH of the solution 3. When about 1/2 of the hydrobromic acid gas was blown in, crystals began to precipitate. The reaction mixture was stirred at 25° C.-35° C. for 1 hour, and at 0° C.-5° C. for 1 hour. The resulting crystals were filtered, washed with cold acetone (167 ml) and dried in vacuo at 50° C.-70° C. (5 Torr-30 Torr) for 3 hours to give citalopram hydrobromide crystals (162 g). The crystals had an HPLC purity of 97.3% (254 nm).

1. customto precipitate
2. waitat 0° C.-5° C. for 1 hour
3. filtrationThe resulting crystals were filtered
4. washwashed with cold acetone (167 ml)
5. customdried in vacuo at 50° C.-70° C. (5 Torr-30 Torr) for 3 hours