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Potassium Carbonate → HCID 53311788, Verbindung

HRID 1401759
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1401759
[CH3:1][C:2]1([CH3:25])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]3[N:15]=[C:16]([N:19]4[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]4)[S:17][CH:18]=3)[CH:5]=[CH:4][C:3]1=2.C([O:29][CH2:30][CH2:31][CH2:32][CH2:33]Br)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[CH3:1][C:2]1([CH3:25])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]2[CH:7]=[C:6]([C:14]3[N:15]=[C:16]([N:19]4[CH2:20][CH2:21][N:22]([CH2:33][CH2:32][CH2:31][CH2:30][OH:29])[CH2:23][CH2:24]4)[S:17][CH:18]=3)[CH:5]=[CH:4][C:3]1=2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 784911-Butanol, 4-bromo-, 1-acetateHCID 53312286HCID 53312286, Verbindung

Produkt 1

HCID 53311788HCID 53311788, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittel
HCID 6344
Dichloromethane
Lösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

120 mg (0.34 mmol) of 1-[4-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)thiazol-2-yl]piperazine were suspended in 3 ml of DMF with 100 μl (0.68 mmol) of 4-bromobutyl acetate and 56 mg (0.41 mmol) of potassium carbonate and stirred at 60° C. overnight. The reaction mixture was taken up in dichloromethane, washed once each with a concentrated sodium hydrogencarbonate solution and a 1N hydrochloric acid solution. The organic phase was dried over sodium sulfate, filtered and evaporated. The protecting group is cleaved off by means of a 1N NaOH solution in methanol: The reaction mixture was stirred at room temperature and subsequently evaporated. The product was purified by means of preparative HPLC and converted into the hydrochloride by treatment with methanolic HCl.

Aufarbeitung

  1. washwashed once each with a concentrated sodium hydrogencarbonate solution
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. stirringThe reaction mixture was stirred at room temperature
  6. customsubsequently evaporated
  7. customThe product was purified by means of preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-31555aa9aa8a4cca9c917947d45d61a8
Quelldatensatz
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08907098B2

Notizen zur Reaktion

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