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Acetic Acid → tert-Butyl methyl(1-((2-(pyrrolidin-1-yl)pyridin-4-yl)methyl)piperidin-4-yl)carbamate

HRID 1193317
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1193317
[CH3:1][N:2]([CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)[C:3](=[O:9])[O:4][C:5]([CH3:8])([CH3:7])[CH3:6].[N:16]1([C:21]2[CH:22]=[C:23]([CH:26]=[CH:27][N:28]=2)[CH:24]=O)[CH2:20][CH2:19][CH2:18][CH2:17]1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>ClCCl>[CH3:1][N:2]([CH:10]1[CH2:11][CH2:12][N:13]([CH2:24][C:23]2[CH:26]=[CH:27][N:28]=[C:21]([N:16]3[CH2:20][CH2:19][CH2:18][CH2:17]3)[CH:22]=2)[CH2:14][CH2:15]1)[C:3](=[O:9])[O:4][C:5]([CH3:8])([CH3:6])[CH3:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 27568064-N-Boc-4-N-Methyl-aminopiperidineHCID 5049666Sodium triacetoxyborohydrideHCID 185258452-(Pyrrolidin-1-yl)isonicotinaldehyde

Produkt 1

HCID 66805506
tert-Butyl methyl(1-((2-(pyrrolidin-1-yl)pyridin-4-yl)methyl)piperidin-4-yl)carbamate
Ausbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

tert-Butyl methyl(piperidin-4-yl)carbamate (2.333 mmol, 1 eq) and 2-(pyrrolidin-1-yl)-isonicotinaldehyde (2.66 mmol, 1.14 eq) were dissolved in dichloromethane (15 ml), and acetic acid (5.459 mmol, 2.34 eq) and sodium triacetoxyborohydride (3.266 mmol, 1.4 eq) were added. The reaction mixture was stirred for 48 h at RT. When the reaction was complete (TLC monitoring), sat. sodium hydrogen carbonate solution was added to the reaction mixture and the phases were separated. The aqueous phase was extracted with dichloromethane (2×30 ml). The combined organic phases were washed with sat. NaCl solution, dried over sodium sulfate and concentrated. The crude product was purified by column chromatography (silica gel, ethyl acetate:cyclohexane 2:1). Yield: 64%.

Aufarbeitung

  1. additionwas added to the reaction mixture
  2. customthe phases were separated
  3. extractionThe aqueous phase was extracted with dichloromethane (2×30 ml)
  4. washThe combined organic phases were washed with sat. NaCl solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe crude product was purified by column chromatography (silica gel, ethyl acetate:cyclohexane 2:1)

Quellen und Nachweise

ORD-Eintrag
ord-95c29457851b41b49df1794a0a560518
Quelldatensatz
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08680159B2

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