Trichloroacetic Acid → 2,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol

HRID 334433

Reaktionsgleichung

Reaktionsgleichung von HRID 334433
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](O)=[O:4].ClC(Cl)(Cl)C([O-])=O.[Na+].[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:30]=[CH:29][C:26](C=O)=[CH:25][CH:24]=2)[CH2:19][CH2:18]1>CN(C)C=O>[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3]([C:26]1[CH:25]=[CH:24][C:23]([N:20]2[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]2)=[CH:30][CH:29]=1)[OH:4]

Komponenten

5

Edukt 3

HCID 6421Trichloroacetic AcidHCID 7365334-(4-Methylpiperazin-1-yl)benzaldehydeHCID 23681045Sodium Trichloroacetate

Produkt 1

HCID 682771722,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanolAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1.0 ml (10.00 mmol) of trichloroacetic acid and, in small portions, 1.854 g. (10 mmol) of sodium 2,2,2-trichloroacetate are added at room temperature to a solution of 1.362 g (6.67 mmol) of 4-(4-methylpiperazine-1-yl)benzaldehyde in 13.5 ml of dimethylformamide. The reaction mixture is stirred for 3 hours at room temperature. The solvent is concentrated and the crude reaction product extracted with ethyl acetate. The organic phase is washed using saturated sodium bicarbonate solution. The organic phases are combined, dried on magnesium sulfate and then concentrated to yield 1.760 g (yield=82%) of 2,2,2-trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol in the form of a white solid.

Aufarbeitung

  1. concentrationThe solvent is concentrated
  2. customthe crude reaction product
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is washed
  5. customdried on magnesium sulfate
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-515ca87369a043708f8648e14abc16e2
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883821B2

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