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Trifluoroacetic acid → [(2S)-2-Methyl-1-piperazinyl]phenylmethanone

HRID 1689959
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1689959
[C:1]([N:9]1[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][C@@H:10]1[CH3:22])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>ClCCl>[CH3:22][C@H:10]1[CH2:11][NH:12][CH2:13][CH2:14][N:9]1[C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:8]
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Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 57581556HCID 57581556, Verbindung

Produkt 1

HCID 57581475[(2S)-2-Methyl-1-piperazinyl]phenylmethanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

(S)-tert-butyl 4-benzoyl-3-methylpiperazine-1-carboxylate (8.16 g, 26.8 mmol) was dissolved in dichloromethane (200 mL). Trifluoroacetic acid (20.7 ml) was added and the reaction was stirred at rt for 1.5 hours. The reaction was quenched into saturated K2CO3 (30 mL) and neutralized by the portion-wise addition of solid NaHCO3. The layers were separated and extracted twice with dichloromethane. The combined organics were dried (MgSO4) and evaporated to give a yellow oil. MS (M+H)+=205.3.

Aufarbeitung

  1. customThe reaction was quenched into saturated K2CO3 (30 mL)
  2. additionneutralized by the portion-wise addition of solid NaHCO3
  3. customThe layers were separated
  4. extractionextracted twice with dichloromethane
  5. dry with materialThe combined organics were dried (MgSO4)
  6. customevaporated
  7. customto give a yellow oil

Quellen und Nachweise

ORD-Eintrag
ord-cb30c2f8c58b427298c22302d42b8756
Quelldatensatz
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08153633B2

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