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Sodium Iodide → 5-(3-(4-(2,3-dichlorophenyl)piperazin-1-yl)propoxy)-1H-benzo[d]imidazol-2(3H)-one

HRID 1750140
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HRID 1750140 반응식
BrC[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:16]=[C:15]2[C:10](C=C[C:13](=[O:17])[NH:14]2)=[CH:9][CH:8]=1.[Na+].[I-].Cl.[Cl:21][C:22]1[C:27]([Cl:28])=[CH:26][CH:25]=[CH:24][C:23]=1[N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1.C([O-])([O-])=O.[K+].[K+].CC#[N:43]>>[Cl:21][C:22]1[C:27]([Cl:28])=[CH:26][CH:25]=[CH:24][C:23]=1[N:29]1[CH2:34][CH2:33][N:32]([CH2:3][CH2:4][CH2:5][O:6][C:7]2[CH:8]=[CH:9][C:10]3[NH:43][C:13](=[O:17])[NH:14][C:15]=3[CH:16]=2)[CH2:31][CH2:30]1
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참가 물질

6

반응물 5

HCID 5238Sodium IodideHCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 107563157-(4-Bromobutoxy)-quinoline-2(1H)-oneHCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride

생성물 1

HCID 565970945-(3-(4-(2,3-dichlorophenyl)piperazin-1-yl)propoxy)-1H-benzo[d]imidazol-2(3H)-one
수율 32%

실험 절차

A mixture of intermediate 48 (110 mg, 0.39 mmol) and NaI (117 mg, 0.78 mmol) in CH3CN was heated to reflux for 30 min and then cooled to rt. Intermediate 41 (156 mg, 0.59 mmol) and anhydrous K2CO3 (215 mg, 1.56 mmol) were added to the mixture. The resulting mixture was heated to reflux and stirred overnight. Precipitated crystals were filtered off and the filtrate was evaporated under reduced pressure. The residue was extracted with EtOAc. The combined EtOAc layers were washed with brine, dried over anhydrous Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with DCM/MeOH=15:1) to give 5-(3-(4-(2,3-dichlorophenyl)piperazin-1-yl)propoxy)-1H-benzo[d]imidazol-2(3H)-one (compound 35) (54 mg, 32%). 1H NMR (300 MHz, CDCl3): δ 9.53 (s, 1H), 9.24 (s, 1H), 7.17-7.13 (m, 2H), 6.97-6.91 (m, 2H), 6.66-6.60 (m, 2H), 3.95 (t, J=5.7 Hz, 2H), 3.20-3.01 (m, 4H), 2.80-2.61 (m, 4H), 2.52 (t, J=7.5 Hz, 2H), 1.82-1.73 (m, 4H). HPLC: 99%, RT 2.325 min. MS (ESI) m/z 435.1 [M+H]+.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 30 min
  3. temperatureThe resulting mixture was heated
  4. temperatureto reflux
  5. customPrecipitated crystals
  6. filtrationwere filtered off
  7. customthe filtrate was evaporated under reduced pressure
  8. extractionThe residue was extracted with EtOAc
  9. washThe combined EtOAc layers were washed with brine
  10. dry with materialdried over anhydrous Na2SO4
  11. concentrationconcentrated in vacuo
  12. custompurified by flash chromatography on silica gel column (elution with DCM/MeOH=15:1)

출처 및 근거

ORD 기록
ord-764a0385a48f4d038a875b82a1e28598
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156822B2

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