Trifluoroacetic acid → N-Methyl-N-(piperidin-4-yl)benzamide

HRID 2168193Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2168193
[CH3:1][N:2]([C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:17])[CH:3]1[CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][CH2:4]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][N:2]([CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)[C:16](=[O:17])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 67977238HCID 67977238, Verbindung

Produkt 1

HCID 12641853N-Methyl-N-(piperidin-4-yl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1,1-dimethylethyl 4-[methyl(phenylcarbonyl)amino]-1-piperidinecarboxylate D14 (1.66 g) was dissolved in DCM (5 mL) then TFA (4.02 mL, 52.1 mmol) was slowly added. The reaction was stirred at room temperature for 30 minutes. TFA and DCM were removed in vacuo. The crude mixture was poured on a top of an Isolute Si—SCX-2 cartridge, eluting with DCM then MeOH then a 2M NH3 in MeOH solution. Fractions containing desired compound were evaporated in vacuo to give title compound D15 in 1.18 g. LCMS [M+H][email protected] min (2 min run)

Aufarbeitung

  1. customTFA and DCM were removed in vacuo
  2. additionThe crude mixture was poured on a top of an Isolute Si—SCX-2 cartridge
  3. washeluting with DCM
  4. additionFractions containing desired compound
  5. customwere evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-fa1f97b294e3473f8c26d1eaebe79171
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09045485B2

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