Sodium Hydroxide → HCID 19978137, Verbindung

HRID 1449526Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1449526
[ClH:1].C([O:4][C:5]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][S:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([C:22]2[S:30][C:25]3=[N:26][CH2:27][CH2:28][CH2:29][N:24]3[C:23]=2[CH2:31][CH2:32][CH3:33])=[O:21])=[CH:15][CH:14]=1)=[O:6])C.[OH-].[Na+]>C(O)C>[ClH:1].[C:5]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][S:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([C:22]2[S:30][C:25]3=[N:26][CH2:27][CH2:28][CH2:29][N:24]3[C:23]=2[CH2:31][CH2:32][CH3:33])=[O:21])=[CH:15][CH:14]=1)([OH:6])=[O:4]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 19978087HCID 19978087, Verbindung

Produkt 1

HCID 19978137HCID 19978137, VerbindungAusbeute 69,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

In 30 ml of ethanol was dissolved 750 mg of N-[4-(5-ethoxycarbonyl-pentylthio)phenyl]-3-propyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carboxamide hydrochloride obtained in Example 89. To the solution was added 3.22 ml of 1N sodium hydroxide aqueous solution, followed by reflux under heating for 2 hours. After cooling the mixture, ethanol was removed under reduced pressure. The aqueous solution was made acidic with consentrated hydrochloric acid, following by removing a little amount of water. To the residue was added isopropylalcohol-diethylether and the precipitated crystals were collected by filtration. This crystals were recrystallized from methanol-diethylether to obtain 494 mg of the titled compound.

Aufarbeitung

  1. temperatureby reflux
  2. temperatureunder heating for 2 hours
  3. customwas removed under reduced pressure
  4. customby removing a little amount of water
  5. additionTo the residue was added isopropylalcohol-diethylether
  6. filtrationthe precipitated crystals were collected by filtration
  7. customThis crystals were recrystallized from methanol-diethylether

Quellen und Nachweise

ORD-Eintrag
ord-6945c9fd101244a49eff35c8db2c9f86
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05599813

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