StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Potassium Carbonate → HCID 59519105, Verbindung

HRID 1161849
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1161849
F[C:2]1[CH:3]=[CH:4][C:5]([N+:18]([O-:20])=[O:19])=[C:6]([CH:17]=1)[C:7]([NH:9][CH2:10][C:11](=[O:16])[NH:12][CH:13]([CH3:15])[CH3:14])=[O:8].[CH3:21][N:22]1[CH2:28][CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH:13]([NH:12][C:11]([CH2:10][NH:9][C:7](=[O:8])[C:6]1[CH:17]=[C:2]([N:25]2[CH2:26][CH2:27][CH2:28][N:22]([CH3:21])[CH2:23][CH2:24]2)[CH:3]=[CH:4][C:5]=1[N+:18]([O-:20])=[O:19])=[O:16])([CH3:15])[CH3:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 2283491-MethylhomopiperazineHCID 44203076HCID 44203076, Verbindung

Produkt 1

HCID 59519105HCID 59519105, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 5-fluoro-N-(isopropylcarbamoylmethyl)-2-nitrobenzamide (INTERMEDIATE IV.1) (400 mg, 1.4 mmol), 1-methylhomopiperazine (0.20 mL, 1.6 mmol) and potassium carbonate (1 g) in acetonitrile (20 mL) were heated at reflux temperature under an Argon atmosphere for 16 h. The mixture was cooled, filtered, the residue washed with DCM (2×1 mL) and the volatiles evaporated under reduced pressure. The red coloured residue was dissolved in DCM (15 mL), washed with 1 N NaOH (aq.) (2×5 mL) and brine (1×5 mL), dried (Na2SO4) and concentrated under reduced pressure to afford N-(isopropylcarbamoylmethyl)-5-(4-methylperhydro-1,4-diazepin-1-yl)-2-nitrobenzamide (510 mg, 1.4 mmol, 100%) as an orange-red solid. This was used in the next step without further purification.

Aufarbeitung

  1. temperaturewere heated
  2. temperatureat reflux temperature under an Argon atmosphere for 16 h
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. washthe residue washed with DCM (2×1 mL)
  6. customthe volatiles evaporated under reduced pressure
  7. dissolutionThe red coloured residue was dissolved in DCM (15 mL)
  8. washwashed with 1 N NaOH (aq.) (2×5 mL) and brine (1×5 mL)
  9. dry with materialdried (Na2SO4)
  10. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-84d5c5e449234e64b23ae00102024938
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07820649B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion