1,4-Dioxane hydrochloride → (R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochloride

HRID 1916416Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1916416
[ClH:1].O1CCOCC1.[F:8][C:9]1([F:32])[C:13]2[N:14]=[CH:15][N:16]=[C:17]([N:18]3[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]3)[C:12]=2[C@H:11]([CH3:31])[CH2:10]1>O1CCOCC1>[ClH:1].[ClH:1].[F:32][C:9]1([F:8])[C:13]2[N:14]=[CH:15][N:16]=[C:17]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[C:12]=2[C@H:11]([CH3:31])[CH2:10]1

Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66845040HCID 66845040, Verbindung

Produkt 1

HCID 66846210(R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochlorideAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4M HCl/dioxane (2.27 mL, 9.09 mmol) was added to a solution of (R)-tert-butyl 4-(7,7-difluoro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazine-1-carboxylate (0.092 g, 0.260 mmol) in dioxane (2 mL.) The reaction mixture was stirred at room temperature overnight, after which it was concentrated to dryness and dried on under high vacuum to give (R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochloride (0.079 g, 93.0% yield) as a solid.

Aufarbeitung

  1. concentrationafter which it was concentrated to dryness
  2. customdried on under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-552e5636f52e4c7a955ca139dada34fc
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08618097B2

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