Potassium Carbonate → HCID 46867019, Verbindung

HRID 2353125Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2353125
[C:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(=O)([O-])[O-].[K+].[K+].[CH3:20][C:21]1[O:25][N:24]=[C:23]([CH2:26]OS(C)(=O)=O)[CH:22]=1>CC#N.O>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][N:11]([CH2:26][C:23]2[CH:22]=[C:21]([CH3:20])[O:25][N:24]=2)[CH2:12][CH2:13]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 57476926Methanesulfonic acid 5-methyl-isoxazol-3-ylmethyl ester

Produkt 1

HCID 46867019HCID 46867019, VerbindungAusbeute 89,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of N-BOC-piperazine (300 mg) in MeCN (5 mL) was added potassium carbonate (289 mg) followed by methanesulfonic acid 5-methyl-isoxazol-3-ylmethyl ester (369 mg). The reaction mixture was heated to reflux for 24 h. After cooling the reaction mixture was diluted with water extracted into ethyl acetate, dried (MgSO4) and the solvent was removed in vacuo to yield 4-(5-methyl-isoxazol-3-ylmethyl)-piperazine-1-carboxylic acid tert-butyl ester (404 mg).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 h
  3. temperatureAfter cooling the reaction mixture
  4. extractionextracted into ethyl acetate
  5. dry with materialdried (MgSO4)
  6. customthe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9c1ac4fe190e4f04a1f61b848aec38b8
Quelldatensatz
uspto-grants-2010_07
Patentnummer
US07750002B2

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