Imipramine Hydrochloride → CID 16052002

HRID 1664118

반응식

HRID 1664118 반응식
[CH:1]1[CH:6]=[C:5]2[CH:7]=[C:8]([C:27]([OH:29])=[O:28])[C:9]([OH:26])=[C:10]([CH2:11][C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH:15]=[C:14]([C:22]([OH:24])=[O:23])[C:13]=3[OH:25])[C:4]2=[CH:3][CH:2]=1.[Na+].[CH3:31][N:32]([CH2:34][CH2:35][CH2:36][N:37]1[C:47]2[CH:48]=[CH:49][CH:50]=[CH:51][C:46]=2[CH2:45][CH2:44][C:43]2[CH:42]=[CH:41][CH:40]=[CH:39][C:38]1=2)[CH3:33].[ClH:52]>O>[CH3:31][N:32]([CH2:34][CH2:35][CH2:36][N:37]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:43]=2[CH2:44][CH2:45][C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][C:47]1=2)[CH3:33].[ClH:52].[CH3:31][N:32]([CH2:34][CH2:35][CH2:36][N:37]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:43]=2[CH2:44][CH2:45][C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][C:47]1=2)[CH3:33].[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[CH:7][C:8]([C:27]([OH:29])=[O:28])=[C:9]([OH:26])[C:10]=2[CH2:11][C:12]2[C:13]([OH:25])=[C:14]([C:22]([OH:24])=[O:23])[CH:15]=[C:16]3[C:21]=2[CH:20]=[CH:19][CH:18]=[CH:17]3)[CH:6]=1

참가 물질

5

반응물 2

HCID 8228Imipramine HydrochlorideHCID 101798076640-22-82회

생성물 2

HCID 8228Imipramine HydrochlorideHCID 16052002CID 16052002수율 92.6%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
41 °C

실험 절차

Synthesis of Imipramine Pamoate-(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).

후처리

  1. customwas prepared at a pH of about 9.5
  2. additionAfter complete addition
  3. customwas continued for approximately 3 additional hours at near 40-42° C.
  4. customthe solid product was isolated by filtration
  5. washwashed with water

출처 및 근거

ORD 기록
ord-2a11bde3d7114fe898ad7f88cd7c27ea
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039461B1

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