Cyclopentanol → Cyclopentyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

HRID 1700365Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1700365
Cl.[Cl:2][C:3]1[CH:4]=[C:5]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]1[CH:10]([C:16]3([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:19][CH2:18][CH2:17]3)[NH:9][CH2:8][CH2:7][C:6]2=1.[CH:25]1(O)[CH2:29]CC[CH2:26]1>O.CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]1[CH:10]([C:16]3([C:20]([O:22][CH:23]4[CH2:29][CH2:25][CH2:26][CH2:24]4)=[O:21])[CH2:17][CH2:18][CH2:19]3)[NH:9][CH2:8][CH2:7][C:6]2=1

Komponenten

5

Edukt 2

HCID 7298CyclopentanolHCID 18317933Ethyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

Produkt 1

HCID 18317862Cyclopentyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11026Titanium isopropoxideKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

4.0 g of the compound of Example 1 are heated at the reflux of 80 ml of cyclopentanol in the presence of 1 ml of titanium tetraisopropoxide. After reaction for 24 hours, the reaction mixture is diluted with water and then filtered. After extraction with dichloromethane, drying and evaporation under reduced pressure, crystallisation of the residue from an ethanol-diethyl ether-hydrogen chloride mixture enables the expected product to be isolated.

Aufarbeitung

  1. customAfter reaction for 24 hours
  2. filtrationfiltered
  3. extractionAfter extraction with dichloromethane
  4. customdrying
  5. customevaporation
  6. customunder reduced pressure, crystallisation of the residue from an ethanol-diethyl ether-hydrogen chloride mixture
  7. customto be isolated

Quellen und Nachweise

ORD-Eintrag
ord-e4421ef6078f48b99198835e66621569
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06350757B1

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