Trifluoroacetic acid → HCID 86660159, Verbindung

HRID 1846757Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1846757
[Cl:1][C:2]1[C:3]([CH:8]2[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)=[N:4][CH:5]=[CH:6][N:7]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[N:4][CH:5]=[CH:6][N:7]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 58547013Tert-butyl 4-(3-chloropyrazin-2-yl)piperidine-1-carboxylate

Produkt 1

HCID 86660159HCID 86660159, VerbindungAusbeute 245,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a well stirred solution of tert-butyl 4-(3-chloropyrazin-2-yl)piperidine-1-carboxylate (92 g, 0.309 mol, 1 eq.) in dichloromethane (1 L) was added trifluoroacetic acid (119 mL, 1.545 mol, 5 eq.). The resulting mixture was heated to reflux overnight (16 h). The mixture was concentrated and the resulting TFA salt was dried with toluene (500 mL) azetropically to give 150 g 2-chloro-3-(piperidin-4-yl)pyrazine. This was used in the next step without further purification.

Aufarbeitung

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux overnight (16 h)
  3. concentrationThe mixture was concentrated
  4. dry with materialthe resulting TFA salt was dried with toluene (500 mL) azetropically

Quellen und Nachweise

ORD-Eintrag
ord-56cee7cd36d54fedaa4e82ed6445d0eb
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952037B2

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