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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
Notes
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Reaction equation

HRID 1750140 reaction equation
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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 5

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

Product 1

HCID 56597094
5-(3-(4-(2,3-dichlorophenyl)piperazin-1-yl)propoxy)-1H-benzo[d]imidazol-2(3H)-one
Yield 32%

Procedure

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]+.

Workup

  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)

Sources & evidence

ORD record
ord-764a0385a48f4d038a875b82a1e28598
Source dataset
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09156822B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes