Potassium Carbonate → HCID 54344233, Verbindung

HRID 1596463

Reaktionsgleichung

Reaktionsgleichung von HRID 1596463
Cl[C:2]([O:4][C:5]([C:8]#[N:9])([CH3:7])[CH3:6])=[O:3].[CH:10]12[CH2:18][CH:14]([CH2:15][NH:16][CH2:17]1)[CH2:13][N:12]([CH2:19][CH:20]([OH:31])[CH2:21][O:22][C:23]1[CH:30]=[CH:29][C:26]([C:27]#[N:28])=[CH:25][CH:24]=1)[CH2:11]2.C([O-])([O-])=O.[K+].[K+]>CC#N>[C:27]([C:26]1[CH:25]=[CH:24][C:23]([O:22][CH2:21][CH:20]([OH:31])[CH2:19][N:12]2[CH2:11][CH:10]3[CH2:18][CH:14]([CH2:15][N:16]([C:2]([O:4][C:5]([C:8]#[N:9])([CH3:7])[CH3:6])=[O:3])[CH2:17]3)[CH2:13]2)=[CH:30][CH:29]=1)#[N:28]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 53254801-Cyano-1-methylethyl chloroformateHCID 217019464-[3-(3,7-Diazabicyclo[3.3.1]non-3-yl)-2-hydroxypropoxy]benzonitrile

Produkt 1

HCID 54344233HCID 54344233, VerbindungAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

1-Cyano-1-methylethyl chloroformate (0.4 g; 1.65 mmol; from step (a) above) was added to a stirred solution of 4-[3-(3,7-diazabicyclo[3.3.1]non-3-yl)-2-hydroxypropoxy]benzonitrile (0.5 g; 1.65 mmol; see Example G above) and K2CO3 (0.7 g) in MeCN (25 mL). The reaction mixture was stirred at 40° C. for 2 h. The salts were filtered off and the filtrate was concentrated and subjected to column chromatography (DCM:MeOH; 19:1) to give the title compound in a 59% yield.

Aufarbeitung

  1. filtrationThe salts were filtered off
  2. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-8a1458b386d24cd3926f094d9ee24c91
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06291475B1

Verknüpfte Notizen

Wird geladen…