反应详情

温度

62 °C

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.

1. custom(>20 min)
2. additionThe reactor and addition funnel
3. washwas rinsed to the reaction with USP water (20.0 g)
4. temperatureThe reaction mixture was heated from about 20° C. to about 50° C. for 1.2 h
5. filtrationSolids were collected by filtration of the mixture at 50° C
6. washResidue was rinsed from the reactor to the
7. filtrationfilter with USP water (4×110.0 g)
8. customAfter drying on the
9. filtrationfilter for 1 h
10. customsolids were dried at about 65° C. to about 78° C. for approximately a day
11. customRecrystallization of imipramine salicylate from a solution of ethanol-water (98/2)
12. customprovided solid, mp 142.2-144.2° C