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Cabergoline → HCID 69068522, Verbindung

HRID 967297
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 967297
[CH3:1][CH2:2][NH:3][C:4]([N:6]([C:13]([C@H:15]1[CH2:30][N:29]([CH2:31][CH:32]=[CH2:33])[C@H:28]2[C@@H:17]([C:18]3[C:23]4[C:24]([CH2:27]2)=[CH:25][NH:26][C:22]=4[CH:21]=[CH:20][CH:19]=3)[CH2:16]1)=[O:14])[CH2:7][CH2:8][CH2:9][N:10]([CH3:12])[CH3:11])=[O:5]>C1(C)C=CC=CC=1>[CH3:1][CH2:2][NH:3][C:4]([N:6]([C:13]([C@H:15]1[CH2:30][N:29]([CH2:31][CH:32]=[CH2:33])[C@H:28]2[C@@H:17]([C:18]3[C:23]4[C:24]([CH2:27]2)=[CH:25][NH:26][C:22]=4[CH:21]=[CH:20][CH:19]=3)[CH2:16]1)=[O:14])[CH2:7][CH2:8][CH2:9][N:10]([CH3:12])[CH3:11])=[O:5].[C:17]1([CH3:16])[CH:28]=[CH:27][CH:24]=[CH:23][CH:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 54746Cabergoline

Produkt 1

HCID 69068522HCID 69068522, VerbindungAusbeute 403,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

The oil obtained by purification on a chromatographic column after the final step of the synthetic path according to the preparation described in Eur. J. Med. Chem., 24, 421, (1989) and containing 100 g of pure cabergoline was dissolved in toluene to give 243 g of a cabergoline toluene solution. The solution was introduced into a reactor pre-cooled at −12[deg.] C., and 182 g of toluene were added to give a 23.5%. w/w cabergoline concentration in this solvent. After cooling again at −12[deg.] C., 362 ml of diethyl ether were added. The mixture was cooled again at −12[deg.] C. and stirred at this temperature for about 17 hours. The obtained precipitate was filtered under vacuum and smoothly dried. The resultant crystal solvate form V was identified by XRD, DSC, IR and NMR, data shown in FIGS. 5-8 respectively.

Aufarbeitung

  1. customThe oil obtained by purification on a chromatographic column after the final step of the synthetic path

Quellen und Nachweise

ORD-Eintrag
ord-55b20bc1f43d4b99b554ac4a5c3cb4d3
Quelldatensatz
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06953854B2

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