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Ethanolamine → HCID 178433882, Verbindung

HRID 386367
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 386367
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[N:32]=[C:31]([CH3:33])/[C:12](=[N:13]/[NH:14][C:15]3[CH:16]=[CH:17][CH:18]=[C:19]([C:22]4[CH:23]=[CH:24][CH:25]=[C:26]([C:28]([OH:30])=[O:29])[CH:27]=4)[C:20]=3[OH:21])/[C:10]2=[O:11])=[CH:6][C:7]=1[CH3:8].O.[CH2:35]([CH2:37][NH2:38])[OH:36]>C1COCC1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[N:32]=[C:31]([CH3:33])/[C:12](=[N:13]/[NH:14][C:15]3[CH:16]=[CH:17][CH:18]=[C:19]([C:22]4[CH:23]=[CH:24][CH:25]=[C:26]([C:28]([OH:30])=[O:29])[CH:27]=4)[C:20]=3[OH:21])/[C:10]2=[O:11])=[CH:6][C:7]=1[CH3:8].[CH2:35]([CH2:37][NH2:38])[OH:36]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 700Ethanolamine2×HCID 962WaterHCID 178433880HCID 178433880, Verbindung

Produkt 1

HCID 178433882HCID 178433882, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Eltrombopag crude orange solid (1 g) was stirred in 16.75 ml of THF at approximately 30° C. Water (2.0 ml) was added slowly so as to maintain a temperature greater then 28° C. When addition was complete, the temperature was returned to 30° C. and the solution filtered through a glass fiber pad (2× Whatman GFC filters) to remove particulate matter. The filter was washed through with THF (2.0 ml) which was added to the filtrate. The filtrate was allowed to cool to room temperature. Ethanolamine (0.324 g, 2.35 mol. equiv.) was dissolved in IMS (26 ml) at 22° C. and stirred under a nitrogen atmosphere at 22° C. The filtrate containing the free acid was added to the ethanolamine solution over 20 to 30 minutes. The resulting dark red suspension was stirred for 3 hours and the solid isolated by filtration and dried at 50° C. in a vacuum oven over night to yield 1.22 g (96%) of the title compound.

Aufarbeitung

  1. temperatureto maintain a temperature greater
  2. custom28° C
  3. additionWhen addition
  4. customwas returned to 30° C.
  5. filtrationthe solution filtered through a glass fiber pad (2× Whatman GFC filters)
  6. customto remove particulate matter
  7. washThe filter was washed through with THF (2.0 ml) which
  8. additionwas added to the filtrate
  9. additionThe filtrate containing the free acid
  10. stirringThe resulting dark red suspension was stirred for 3 hours
  11. customthe solid isolated by filtration
  12. customdried at 50° C. in a vacuum oven over night

Quellen und Nachweise

ORD-Eintrag
ord-1527ce0e769b4b319fec687efe074ce9
Quelldatensatz
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08372822B2

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