Potassium Carbonate → HCID 46867019, Verbindung

HRID 1689884Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1689884
[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-bab7f3ee5a124b4aaa179b97b3e2225f
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08153629B2

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