Imipramine → CID 16052002

Participants

Reaction Conditions

Reaction Steps

Synthesis of Imipramine Pamaote—(Form VI)— A solution of disodium pamoate (43.88 g) in water (446.0 g) was prepared at a pH of about 9.5. A solution of imipramine HCl (63.38 g) in water (485.0 g) was prepared at a pH of about 4.0. The imipramine HCl solution (552.7 g) was added to the disodium pamoate solution at a controlled rate over a period of about 2.5 hours. After complete addition, the mixture was warmed to near 40-42° C. over approximately 4 h. Stirring was continued for approximately 3 additional hours at near 40-42° C. and then the solid product was isolated by filtration and washed with water. Imipramine pamoate (85.22 g) (92.6%) was isolated after drying at (78-80° C.). Throughout the heating process, samples were taken from the mixture and washed with water then dried. The Imipramine pamoate samples isolated at 42° C. (1.25 h) and 42° C. (2.25 h) contained a mixture of amorphous Imipramine Pamoate and Form VI. The Imipramine pamoate solid was characterized by PXRD (FIG. 18), FTIR (FIG. 19) and DSC (FIG. 20).

Provenance & Evidence