Sodium Iodide → Aripiprazole

HRID 503827

反応式

HRID 503827 の反応式
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

参加物

8

反応物 4

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

生成物 1

HCID 60795Aripiprazole収率 159.6%

試薬・触媒・溶媒 3

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-07502c785a674e6b88dc91d2c05aded7
出典データセット
uspto-grants-2010_08
特許番号
US07777039B2

関連ノート

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