Hydrochloric Acid → N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochloride

HRID 2077964Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2077964
[CH2:1]([NH:3][C:4]([C:6]1[C:11]([F:12])=[CH:10][C:9]([N:13]2[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]2)=[C:8]([F:26])[CH:7]=1)=[O:5])[CH3:2].[ClH:27]>O1CCOCC1.C(OCC)C>[ClH:27].[CH2:1]([NH:3][C:4](=[O:5])[C:6]1[CH:7]=[C:8]([F:26])[C:9]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:10][C:11]=1[F:12])[CH3:2]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 58324386HCID 58324386, Verbindung

Produkt 1

HCID 66775087N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochlorideAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

tert-butyl 4-(4-(ethylcarbamoyl)-2,5-difluorophenyl)piperazine-1-carboxylate (0.020 g, 0.054 mmol) was diluted with 4.0M HCl in dioxane (3 mL) and stirred for 30 min. The thick white precipitate that formed was diluted with ethyl ether (10 mL) and stirred until a fine suspension resulted. The precipitate was filtered under nitrogen and dried in vacuum to afford N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochloride (16.2 mg, 0.053 mmol, 98% yield) as a white solid. ESI-MS:m/z 270 (M+H)+.

Aufarbeitung

  1. customThe thick white precipitate that formed
  2. stirringstirred until a fine suspension
  3. customresulted
  4. filtrationThe precipitate was filtered under nitrogen
  5. customdried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4cfbda88a33b4d94837aeb0fe662feea
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928105B2

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