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Water → HCID 22048232, Verbindung

HRID 1830610
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1830610
[ClH:1].[CH2:2]([N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][N:14]=2)[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH2:23][CH2:24][CH2:25][OH:26])[CH:17]=2)=[C:8]([NH:27][C:28]([NH:30][C:31]2[C:36]([CH:37]([CH3:39])[CH3:38])=[CH:35][C:34]([NH2:40])=[CH:33][C:32]=2[CH:41]([CH3:43])[CH3:42])=[O:29])[C:7]1=[O:44])[CH2:3][CH2:4][CH3:5].O>CO>[OH2:22].[ClH:1].[CH2:2]([N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][N:14]=2)[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH2:23][CH2:24][CH2:25][OH:26])[CH:17]=2)=[C:8]([NH:27][C:28]([NH:30][C:31]2[C:32]([CH:41]([CH3:43])[CH3:42])=[CH:33][C:34]([NH2:40])=[CH:35][C:36]=2[CH:37]([CH3:39])[CH3:38])=[O:29])[C:7]1=[O:44])[CH2:3][CH2:4][CH3:5]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 962WaterHCID 10282637Urea, N-[4-amino-2,6-bis(1-methylethyl)phenyl]-N'-[1-butyl-1,2-dihydro-4-[3-(3-hydroxypropoxy)phenyl]-2-oxo-1,8-naphthyridin-3-yl]-, hydrochloride (1:1)

Produkt 1

HCID 22048232HCID 22048232, VerbindungAusbeute 136,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A suspension of an amorphous solid of N-[1-butyl-4-[3-[3-(hydroxy)propoxy]phenyl]-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N′-(2,6-diisopropyl-4-aminophenyl)urea hydrochloride (125 g) in methanol (375 ml) was stirred with heating at about 60° C. to dissolve the solid. Water (3.7 ml) was added thereto, and the mixture was stirred for 15 minutes, and filtered while the mixture was hot. The filtrate was stirred at 40° C. to 50° C. for about 2 hours, and then allowed to stand for cooling. The mixture was stirred at room temperature for 14 hours, and then stirred under ice-cooling for 2 hours. The precipitated crystals were collected by filtration to give the title compound as colorless crystals (87.5 g).

Aufarbeitung

  1. dissolutionto dissolve the solid
  2. stirringthe mixture was stirred for 15 minutes
  3. filtrationfiltered while the mixture
  4. stirringThe filtrate was stirred at 40° C. to 50° C. for about 2 hours
  5. temperaturefor cooling
  6. stirringThe mixture was stirred at room temperature for 14 hours
  7. stirringstirred under ice-
  8. temperaturecooling for 2 hours
  9. filtrationThe precipitated crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-121c8261abac4af99760cec554ea8de8
Quelldatensatz
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07067528B2

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