Sodium Iodide → Aripiprazole

HRID 503827

반응식

HRID 503827 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][CH2:12][C:13](=[O:17])[NH:14]2)=[CH:9][CH:8]=1.[I-].[Na+].C([O-])([O-])=O.[K+].[K+].Cl.[Cl:27][C:28]1[C:33]([Cl:34])=[CH:32][CH:31]=[CH:30][C:29]=1[N:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1>C(#N)C.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[CH:31]1[CH:30]=[C:29]([N:35]2[CH2:40][CH2:39][N:38]([CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]3[CH:8]=[CH:9][C:10]4[CH2:11][CH2:12][C:13](=[O:17])[NH:14][C:15]=4[CH:16]=3)[CH2:37][CH2:36]2)[C:28]([Cl:27])=[C:33]([Cl:34])[CH:32]=1

참가 물질

8

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 104674677-(4-Chlorobutoxy)-1,2,3,4-tetrahydroquinolin-2-oneHCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride

생성물 1

HCID 60795Aripiprazole수율 159.6%

시약·촉매·용매 3

HCID 74236Tetrabutylammonium Bromide촉매HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A mixture of 100 gm 7-(4-chloro butoxy)-3,4-Dihydrocarbostyril in 600 ml acetonitrile with sodium iodide (88.6 gm), K2CO3 (109 gm), Tetrabutylammonium bromide (TBAB) (0.5 gm) and 1-(2,3-dichlorophenyl)piperazine hydrochloride (110 gm) was stirred at ambient temperature. The reaction mixture was refluxed and maintained at reflux until reaction completes. The reaction mass was cooled at room temperature. DM Water (500 ml) was added to reaction mass and stirred for 30 min at ambient temperature. The mass was filtered and washed with water till pH of filtrate came to 7.0-7.5. The solid was dried in hot air oven at 60° C. to give Aripiprazole.

후처리

  1. temperatureThe reaction mixture was refluxed
  2. temperaturemaintained
  3. temperatureat reflux until reaction completes
  4. temperatureThe reaction mass was cooled at room temperature
  5. stirringstirred for 30 min at ambient temperature
  6. filtrationThe mass was filtered
  7. washwashed with water till pH of filtrate
  8. customThe solid was dried in hot air oven at 60° C.

출처 및 근거

ORD 기록
ord-07502c785a674e6b88dc91d2c05aded7
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07777039B2

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