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Water → HCID 66696142, Verbindung

HRID 69116
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 69116
[C:1]1([C@@H:7]2[NH:12][CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[CH3:22][O:23][CH2:24][CH2:25]Br.O>CN(C=O)C.C(OCC)(=O)C>[CH3:22][O:23][CH2:24][CH2:25][N:12]1[CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8][C@@H:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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Komponenten

7

Edukt 4

HCID 962WaterHCID 24758Sodium hydride2×HCID 809722-Bromoethyl methyl ether2×HCID 7173868rel-tert-butyl (3R)-3-phenylpiperazine-1-carboxylate

Produkt 1

HCID 66696142HCID 66696142, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228
Dimethylformamide
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere, to a solution of 330 mg of tert-butyl (3S)-3-phenylpiperazine-1-carboxylate in 3.5 mL of DMF was added 75.4 mg of sodium hydride (including 40% mineral oil) under ice-cooling, followed by stirring for 30 minutes. To the mixture was added 0.27 mL of 2-bromoethyl methyl ether, followed by stirring at room temperature for 16 hours. To the mixture were added 75.4 mg of sodium hydride (including 40% mineral oil) and 0.6 mL of 2-bromoethyl methyl ether, followed by further stirring for 8 hours. The mixture was poured into a mixture of water and ethyl acetate, and the aqueous layer was separated. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 330 mg of tert-butyl (3S)-4-(2-methoxyethyl)-3-phenylpiperazine-1-carboxylate.

Aufarbeitung

  1. temperaturecooling
  2. stirringby stirring at room temperature for 16 hours
  3. stirringby further stirring for 8 hours
  4. customthe aqueous layer was separated
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe residue was purified by silica gel column chromatography (chloroform/methanol)

Quellen und Nachweise

ORD-Eintrag
ord-675fb810c858404ba863909b3ae8a4db
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08822448B2

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