Potassium Carbonate → HCID 178491756, Verbindung

HRID 1517386Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1517386
Cl[CH2:2][C:3]1[C:8]2[NH:9][C:10]([CH2:12][N:13]([CH3:27])[S:14]([C:17]3[C:22]([CH3:23])=[CH:21][C:20]([O:24][CH3:25])=[CH:19][C:18]=3[CH3:26])(=[O:16])=[O:15])=[N:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].Cl.Cl.[N:36]1[CH:41]=[CH:40][C:39]([N:42]2[CH2:52][CH2:51][C:45]3([CH2:50][CH2:49][NH:48][CH2:47][CH2:46]3)[CH2:44][CH2:43]2)=[CH:38][CH:37]=1>CC(C)=O>[CH3:25][O:24][C:20]1[CH:21]=[C:22]([CH3:23])[C:17]([S:14]([N:13]([CH3:27])[CH2:12][C:10]2[NH:9][C:8]3[C:3]([CH2:2][N:48]4[CH2:47][CH2:46][C:45]5([CH2:51][CH2:52][N:42]([C:39]6[CH:40]=[CH:41][N:36]=[CH:37][CH:38]=6)[CH2:43][CH2:44]5)[CH2:50][CH2:49]4)=[CH:4][CH:5]=[CH:6][C:7]=3[N:11]=2)(=[O:16])=[O:15])=[C:18]([CH3:26])[CH:19]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 66701057HCID 66701057, VerbindungHCID 178491755HCID 178491755, Verbindung

Produkt 1

HCID 178491756HCID 178491756, VerbindungAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of N-((7-(chloromethyl)-1H-benzo[d]imidazol-2-yl)methyl)-4-methoxy-N,2,6-trimethylbenzenesulfonamide (0.74 mmol, 1.0 eq.), K2CO3 (2.5 eq.) and 9-pyridin-4-Yl-3,9-diazaspiro[5.5]undecane dihydrochloride (AMN-01) (0.88 mmol, 1.2 eq.) in abs. acetone (20 ml) was heated under reflux for 16 h. The reaction mixture was filtered off and the filtrate was concentrated in order to obtain the crude product, which was purified by column chromatography over neutral aluminium oxide. Yield: 25%

Aufarbeitung

  1. temperatureunder reflux for 16 h
  2. filtrationThe reaction mixture was filtered off
  3. concentrationthe filtrate was concentrated in order

Quellen und Nachweise

ORD-Eintrag
ord-42392fb438ee4f46b74ff7662e8b6d32
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08232288B2

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