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Example 8; Preparation of Imipramine SalicylateSodium Salicylate (16.4 g) in USP water (118.0 g) was stirred at 20 C. in a 1 L reactor. After 15 min, the solution was checked and exhibited pH 6.23. In a Imipramine HCl (31.7 g) in USP water (320.0 g) was stirred at 22 C. in a 500 mL reactor until a solution was observed (>20 min). The Imipramine HCl solution was checked and exhibited a pH 4.54. The Imipramine HCl solution was added via metered addition funnel to the sodium salicylate solution at 20 C. over 1.75 h. The reactor and addition funnel was rinsed to the reaction with USP water (20.0 g). The reaction mixture was heated from about 20 C. to about 50 C. for 1.2 h. The mixture was heated to about 62 C. for 17 h. Solids were collected by filtration of the mixture at 50 C. Residue was rinsed from the reactor to the filter with USP water (4×110.0 g). After drying on the filter for 1 h, solids were dried at about 65 C. to about 78 C. for approximately a day. Imipramine salicylate, mp 141-143.6 C. (39.8 g, 95.1%). Recrystallization of imipramine salicylate from a solution of ethanol-water (98/2) provided solid, mp 142.2-144.2 C. The DSC thermogram (FIG. 16), FTIR analysis (FIG. 17) and 1H NMR spectra (FIG. 18) were consistent with the expected structure.
95.1%
In water; at 20 - 62℃; for 19.95h;
Sodium Salicylate (16.4 g) in USP water (118.0 g) was stirred at 20 C. in a 1 L reactor. After 15 min, the solution was checked and exhibited pH 6.23. In a Imipramine HCl (31.7 g) in USP water (320.0 g) was stirred at 22 C. in a 500 mL reactor until a solution was observed (>20 min). The Imipramine HCl solution was checked and exhibited a pH 4.54. The Imipramine HCl solution was added via metered addition funnel to the sodium salicylate solution at 20 C. over 1.75 h. The reactor and addition funnel was rinsed to the reaction with USP water (20.0 g). The reaction mixture was heated from about 20 C. to about 50 C. for 1.2 h. The mixture was heated to about 62 C. for 17 h. Solids were collected by filtration of the mixture at 50 C. Residue was rinsed from the reactor to the filter with USP water (4×110.0 g). After drying on the filter for 1 h, solids were dried at about 65 C. to about 78 C. for approximately a day. Imipramine salicylate, mp 141-143.6 C. (39.8 g, 95.1%). Recrystallization of imipramine salicylate from a solution of ethanol-water (98/2) provided solid, mp 142.2-144.2 C. The DSC thermogram (FIG. 16), FTIR analysis (FIG. 17) and 1H NMR spectra (FIG. 18) were consistent with the expected structure
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