Sodium Iodide → Aripiprazole

HRID 239004

반응식

HRID 239004 반응식
Br[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(#N)C.[Cl:23][C:24]1[C:29]([Cl:30])=[CH:28][CH:27]=[CH:26][C:25]=1[N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:23][C:24]1[C:29]([Cl:30])=[CH:28][CH:27]=[CH:26][C:25]=1[N:31]1[CH2:36][CH2:35][N:34]([CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]2[CH:16]=[C:15]3[C:10]([CH2:11][CH2:12][C:13](=[O:17])[NH:14]3)=[CH:9][CH:8]=2)[CH2:33][CH2:32]1

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 6342AcetonitrileHCID 8518331-(2,3-Dichlorophenyl)piperazineHCID 105420647-(4-bromobutoxy)-3,4-dihydro-2(1H)-quinolinone

생성물 1

HCID 60795Aripiprazole수율 80.8%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 8471Triethylamine용매

실험 절차

A suspension of 47 g of 7-(4-bromobutoxy)-3,4-dihydrocarbostyril, 35 g of sodium iodide with 600 ml of acetonitrile was refluxed for 30 minutes. To this suspension was added 40 g of 1-(2,3-dichlorophenyl)piperazine and 33 ml of triethylamine and the whole mixture was further refluxed for 3 hours. After the solvent was removed by evaporation, the residue thus obtained was dissolved in chloroform, washed with water then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation, and the residue thus obtained was recrystallized from ethanol twice, to yield 57.1 g of 7-{4-[4-(2,3-dichlorophenyl)-1-piperazinyl]butoxy}-3,4-dihydrocarbostyril.

후처리

  1. temperaturewas refluxed for 30 minutes
  2. temperaturethe whole mixture was further refluxed for 3 hours
  3. customAfter the solvent was removed by evaporation
  4. customthe residue thus obtained
  5. washwashed with water
  6. dry with materialthen dried with anhydrous magnesium sulfate
  7. customThe solvent was removed by evaporation
  8. customthe residue thus obtained
  9. customwas recrystallized from ethanol twice

출처 및 근거

ORD 기록
ord-a18fbd88147b417a889e11d3c18f357c
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642760B2

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