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1,4-Dioxane hydrochloride → HCID 67339956, Verbindung

HRID 82390
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 82390
[ClH:1].O1CCOCC1.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C@H:15]([C:25]([N:27]2[CH2:32][CH2:31][N:30]([C:33]3[C:34]4[C@H:41]([CH3:42])[CH2:40][CH2:39][C:35]=4[N:36]=[CH:37][N:38]=3)[CH2:29][CH2:28]2)=[O:26])[CH2:16][NH:17]C(=O)OC(C)(C)C)=[CH:11][CH:10]=1>O1CCOCC1>[ClH:8].[ClH:1].[NH2:17][CH2:16][C@H:15]([C:12]1[CH:13]=[CH:14][C:9]([Cl:8])=[CH:10][CH:11]=1)[C:25]([N:27]1[CH2:28][CH2:29][N:30]([C:33]2[C:34]3[C@H:41]([CH3:42])[CH2:40][CH2:39][C:35]=3[N:36]=[CH:37][N:38]=2)[CH2:31][CH2:32]1)=[O:26]
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Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86618948tert-butyl (S)-2-(4-chlorophenyl)-3-(4-((R)-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate

Produkt 1

HCID 67339956HCID 67339956, VerbindungAusbeute 157,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4M HCl/dioxane (0.860 ml, 3.44 mmol) was added to a solution of tert-butyl (S)-2-(4-chlorophenyl)-3-(4-((R)-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate (0.043 g, 0.0860 mmol) in dioxane (1.2 mL). The reaction mixture was stirred at room temperature overnight (16 hours), after which it was concentrated and dried on high vacuum line. The resulting residue was dissolved in minimal MeOH, and the product was triturated by the addition of ether. The resulting solids were isolated by filtration through Varian quantitative membrane filter paper with nitrogen pressure, rinsed with ether, dried with nitrogen pressure, and further dried in vacuo to give (S)-3-amino-2-(4-chlorophenyl)-1-(4-((R)-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazin-1-yl)propan-1-one dihydrochloride (0.032 g, 78.7% yield) as a white powder. LC/MS (APCI+) m/z 400 [M+H]+.

Aufarbeitung

  1. concentrationafter which it was concentrated
  2. customdried on high vacuum line
  3. dissolutionThe resulting residue was dissolved in minimal MeOH
  4. customthe product was triturated by the addition of ether
  5. customThe resulting solids were isolated by filtration through Varian quantitative membrane
  6. filtrationfilter paper with nitrogen pressure
  7. washrinsed with ether
  8. customdried with nitrogen pressure
  9. customfurther dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bdd42226ae12433abf0c4db17e146b67
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08846681B2

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