Acetone → 5-[(3-Phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride

HRID 1489152Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1489152
[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:27].CC(C)=O>C(O)C.C(OCC)(=O)C>[ClH:27].[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

6

Edukt 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 98410295-(3-Phenylindolin-1-ylcarbonyl)-4,5,6,7-tetrahydrobenzimidazole

Produkt 1

HCID 104298255-[(3-Phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A 100 mg portion of the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole produced in the preferred embodiment 3 was dissolved in 5 ml ethanol, and 0.5 ml of a 4N hydrogen chloride solution in ethyl acetate was added under ice cooling, after which concentration under reduced pressure gave an oily residue. Five ml of acetone was added to precipitate crystals which were collected by filtration. The crystals were dissolved in 1 ml of water and then reconcentrated under reduced pressure and thoroughly dried to obtain the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride (compound 4) listed in the above heading.

Aufarbeitung

  1. concentrationafter which concentration under reduced pressure
  2. customgave an oily residue
  3. customto precipitate crystals which
  4. filtrationwere collected by filtration
  5. dissolutionThe crystals were dissolved in 1 ml of water
  6. customthoroughly dried

Quellen und Nachweise

ORD-Eintrag
ord-542bd7980204498e812331bb63cc3354
Quelldatensatz
uspto-grants-1997_10
Patentnummer
US05677326

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