Potassium Carbonate → HCID 10139190, Verbindung

HRID 1181325Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1181325
C([O:4][C:5]1[CH:6]=[C:7]([O:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[N:22]([CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]4)[C:21]4[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=4[N:19]=3)=[CH:14][CH:13]=2)[CH:8]=[CH:9][CH:10]=1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O1CCCC1>[CH:23]1([N:22]2[C:21]3[CH:29]=[CH:30][C:31]([C:33]([O:35][CH2:36][CH3:37])=[O:34])=[CH:32][C:20]=3[N:19]=[C:18]2[C:15]2[CH:14]=[CH:13][C:12]([O:11][C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([OH:4])[CH:6]=3)=[CH:17][CH:16]=2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

Komponenten

5

Edukt 2

HCID 11430Potassium CarbonateHCID 10228675HCID 10228675, Verbindung

Produkt 1

HCID 10139190HCID 10139190, VerbindungAusbeute 97,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ethyl 2-[4-(3-acetoxyphenyloxy)phenyl]-1-cyclohexylbenzimidazole-5-carboxylate (87 g) obtained in Example 27 was dissolved in methyl alcohol (250 ml) and tetrahydrofuran (250 ml), and potassium carbonate (31 g) was added. The mixture was stirred for 30 min at room temperature. The insoluble materials were filtered off and the filtrate was concentrated under reduced pressure. Water was added to the residue and the mixture was neutralized with 2N hydrochloric acid. The precipitated crystals were collected by filtration to give the title compound (78 g, yield 97%).

Aufarbeitung

  1. filtrationThe insoluble materials were filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionWater was added to the residue
  4. filtrationThe precipitated crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-0e06dde6754e496c88b8bb3249bd7b5b
Quelldatensatz
uspto-grants-2007_10
Patentnummer
US07285551B2

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