Phenylacetic Acid → 2,5-Dimethyl-1-(phenylacetyl)-piperazine

HRID 38272

Reaktionsgleichung

Reaktionsgleichung von HRID 38272
C(N(C(C)C)CC)(C)C.[CH3:10][C@H:11]1[CH2:16][NH:15][C@H:14]([CH3:17])[CH2:13][NH:12]1.[C:18]1([CH2:24][C:25](O)=[O:26])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.O>[CH3:10][CH:11]1[CH2:16][NH:15][CH:14]([CH3:17])[CH2:13][N:12]1[C:25](=[O:26])[CH2:24][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Komponenten

7

Edukt 4

HCID 999Phenylacetic AcidHCID 81531DiisopropylethylamineHCID 2206722,5-Dimethylpiperazine, trans-HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

Produkt 1

HCID 649793942,5-Dimethyl-1-(phenylacetyl)-piperazineAusbeute 178,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Diisopropylethylamine (0.38 ml) was added to a solution of trans-2,5-dimethyl-piperazine (1.50 g), phenyl acetic acid (0.59 g) and HATU (1.55 g) in DMF (10 ml). The reaction mixture was stirred overnight at ambient temperature. The solution was diluted with water, then extracted with ethyl acetate. The organic extracts were dried (MgSO4) then concentrated in vacuo to give the sub-title compound (1.8 g).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic extracts were dried (MgSO4)
  3. concentrationthen concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-715e1f13ccc9473e8841e52835088166
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524715B2

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