Trifluoroacetic acid → (R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate

HRID 80755Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 80755
[C:1]([N:4]1[CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[C@H:6]([CH3:17])[CH2:5]1)(=[O:3])[CH3:2].[C:18]([OH:24])([C:20]([F:23])([F:22])[F:21])=[O:19]>C(Cl)Cl>[F:21][C:20]([F:23])([F:22])[C:18]([OH:24])=[O:19].[CH3:17][C@H:6]1[NH:7][CH2:8][CH2:9][N:4]([C:1](=[O:3])[CH3:2])[CH2:5]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 86690247HCID 86690247, Verbindung

Produkt 1

HCID 86690248(R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetateAusbeute 137,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of (R)-tert-butyl 4-acetyl-2-methylpiperazine-1-carboxylate (1.34 g, 5.53 mmol) and TFA (10 mL, 130 mmol) in DCM (30 mL) was stirred at rt for 45 min, then concentrated, diluted with DCM, and then concentrated again which was repeated 3 times. Dried under high vacuum at 80° C. to give (R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate (1.95 g). MS (ESI+) m/z 143.0 (M+H)+.

Aufarbeitung

  1. concentrationconcentrated
  2. additiondiluted with DCM
  3. concentrationconcentrated again which
  4. customDried under high vacuum at 80° C.

Quellen und Nachweise

ORD-Eintrag
ord-70d07e067fa340f483a5e47aede96369
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846656B2

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