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2-{(3,4-Dihydroxy-phenyl)-[3-hydroxy-4-oxo-cyclohexa-2,5-dien-(E)-ylidene]-methyl}-benzenesulfonic acid; compound with [3-(10,11-dihydro-dibenzo[b,f]azepin-5-yl)-propyl]-dimethyl-amine[ No CAS ]
Example 7; Preparation of Imipramine XinafoateTo a solution containing 7.7 g of 3-hydroxy-2-napthoic acid in 75.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 9.4. To a second solution of 13.6 g of <strong>[113-52-0]imipramine HCl</strong> in 100.0 g of USP water was added as necessary dilute HCl or NaOH solution to adjust the solution to about pH 4.5. The <strong>[113-52-0]imipramine HCl</strong> solution was added to the 3-hydroxy-2-napthoic sodium salt solution over a period of about 2 h. The mixture was stirred and held at around 50 C. for at least 18 h. The mixture was cooled to below 25 C. and the solids were collected by filtration. The solid cake was washed with USP water (2×100 g). The solid cake was dried at 105 C. under vacuum to yield a powder (12.7 g) and characterized by DSC (FIG. 13), FTIR (FIG. 14) and 1H NMR (FIG. 15).
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
Disodium pamoate (68.21 g) was dissolved in 800 ml of water and the solution is poured slowly into a solution of 100 g of <strong>[113-52-0]imipramine hydrochloride</strong> in a mixture of 200 ml of water and 1000 ml of acetone at 50-55C. The contents were cooled slowly to room temperature, stirred to commence crystallization and then filtered. <n="7"/>The solid mass was poured into distilled water (2 liters), stirred, filtered and washed with water. The product was added in water (2 liters) and heated to 65-70C. The contents were cooled to 40-45C, filtered, washed with water and then dried under reduced pressure at about 70C till moisture content was less than 1.0%
In water; at 5℃;
lmipramine hydrochloride (20 g) was dissolved in 100 ml of water and the solution is poured slowly into a solution of 13.66 g of disodium pamoate in 300 ml of water. The contents were cooled to 5-10C and then filtered. The solid was washed with 1.4 liter of distilled water and then dried under reduced pressure at about 70C till moisture content was less than 2.0%.
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