Potassium Hydroxide → HCID 68704398, Verbindung

HRID 222131Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 222131
C([O:3][C:4]([C:6]1[C:10]2[CH2:11][CH2:12][C:13]3[C:18]([C:9]=2[N:8]([CH3:20])[CH:7]=1)=[N:17][C:16]([NH2:19])=[N:15][CH:14]=3)=[O:5])C.[OH-].[K+]>CCO>[NH2:19][C:16]1[N:17]=[C:18]2[C:13]([CH2:12][CH2:11][C:10]3[C:6]([C:4]([OH:5])=[O:3])=[CH:7][N:8]([CH3:20])[C:9]=32)=[CH:14][N:15]=1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 687069418-Amino-1-methyl-4,5-dihydro-1H-1,7,9-triaza-cyclopenta[a]naphthalene-3-carboxylic acid ethyl ester

Produkt 1

HCID 68704398HCID 68704398, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 8-amino-1-methyl-4,5-dihydro-1H-1,7,9-triaza -cyclopenta[a]naphthalene-3-carboxylic acid ethyl ester M1 (0.51 mmol) in 95% EtOH (10 mL), KOH (1.54 mmol) was added. The mixture was heated to reflux for 10 h then cooled and evaporated to dryness. The residue was dissolved in 30 mL of water, acidified with glacial AcOH and the precipitate was filtered and washed with water. The product was dried affording the title compound (75% yield). ESI (+) MS: m/z 245 (MH+). 1H NMR: 2.65 (t, J=7.80, 2H), 2.92 (t, J=7.80, 2H), 4.15 (s, 3H), 6.39 (bs, 2H), 7.78 (s, 1H), 8.01 (s, 1H), 12.30 (bs, 1H).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 10 h
  3. temperaturethen cooled
  4. customevaporated to dryness
  5. dissolutionThe residue was dissolved in 30 mL of water
  6. filtrationthe precipitate was filtered
  7. washwashed with water
  8. customThe product was dried

Quellen und Nachweise

ORD-Eintrag
ord-215babdb15ec4e4e83c15f898fcbbc20
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08207180B2

Notizen zur Reaktion

Wird geladen…