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Methanol → N-(1H-Indol-4yl)-N'-methyl-N-phenyl-ethane-1,2-diamine

HRID 268765
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 268765
[NH:1]1[C:9]2[C:4](=[C:5]([N:10]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:11](=O)[CH2:12][NH:13][CH3:14])[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.S(C)C.CO.C([O-])(O)=O.[Na+]>C1COCC1.Cl.CCOC(C)=O>[NH:1]1[C:9]2[C:4](=[C:5]([N:10]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:11][CH2:12][NH:13][CH3:14])[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 887MethanolHCID 1068Dimethyl Sulfide2×HCID 516892Sodium BicarbonateHCID 59831661N-(1H-Indol-4-yl)-2-methylamino-N-phenyl-acetamide

Produkt 1

HCID 17747554N-(1H-Indol-4yl)-N'-methyl-N-phenyl-ethane-1,2-diamine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313
Hydrochloric Acid
Katalysator
HCID 8028TetrahydrofuranLösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a room temperature solution of N-(1H-indol-4-yl)-2-methylamino-N-phenyl-acetamide XXIV (122 mg, crude 0.435 mmol) in THF (6 ml) was added BH3.SMe2 (2 M in THF, 653 μl, 1.31 mmol). The mixture was stirred at room temperature for 2 hours, at 50° C. for 2 hours, and at reflux for 2 hours. The resulting mixture was then kept at −18° C. for 5 days. It was then warmed at room temperature and BH3.SMe2 (2M in THF, 653 μl, 1.31 mmol) was added. The mixture was refluxed for 45 minutes, cooled to 0° C., and MeOH (1.5 ml) and HCl (conc., 9 drops) were added. The mixture was stirred at 0° C. for 5 minutes, at room temperature for 1 hour and at 50° C. for 2 hours. The reaction mixture was cooled to room temperature and diluted a saturated solution of NaHCO3 and EtOAc. The aqueous layer was extracted with EtOAc. The combined organic layers were dried over Na2SO4, filtered, concentrated, and purified via flash chromatography (DCM/MeOH/NH4OH). The chromatographed material was dissolved in p-xylene (9 ml) and Pd/C (5%, 14 mg) was added. The reaction mixture was refluxed for 3 hours, cooled to room temperature, and filtered through a celite pad with the aid of hot methanol. The filtrate was concentrated and purified via flash chromatography (DCM/MeOH/NH4OH) affording N-(1H-indol-4yl)-N′-methyl-N-phenyl-ethane-1,2-diamine XXV (8 mg, light brown oil). MS (M+H)=266.

Aufarbeitung

  1. temperatureat reflux for 2 hours
  2. waitThe resulting mixture was then kept at −18° C. for 5 days
  3. temperatureIt was then warmed at room temperature
  4. temperatureThe mixture was refluxed for 45 minutes
  5. temperaturecooled to 0° C.
  6. stirringThe mixture was stirred at 0° C. for 5 minutes, at room temperature for 1 hour and at 50° C. for 2 hours
  7. temperatureThe reaction mixture was cooled to room temperature
  8. extractionThe aqueous layer was extracted with EtOAc
  9. dry with materialThe combined organic layers were dried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. custompurified via flash chromatography (DCM/MeOH/NH4OH)
  13. dissolutionThe chromatographed material was dissolved in p-xylene (9 ml)
  14. additionPd/C (5%, 14 mg) was added
  15. temperatureThe reaction mixture was refluxed for 3 hours
  16. temperaturecooled to room temperature
  17. filtrationfiltered through a celite pad with the aid of hot methanol
  18. concentrationThe filtrate was concentrated
  19. custompurified via flash chromatography (DCM/MeOH/NH4OH)

Quellen und Nachweise

ORD-Eintrag
ord-b478bae726b1458ab14707f7dd1002cf
Quelldatensatz
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07446118B2

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