HCID 59605970, Verbindung → (4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanone

HRID 1945493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1945493
C(OC([N:8]1[CH2:13][CH2:12][C:11]([CH3:21])([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C>C(O)(C(F)(F)F)=O.C(Cl)Cl.O>[CH3:21][C:11]1([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

Komponenten

5

Edukt 1

HCID 59605970HCID 59605970, Verbindung

Produkt 1

HCID 24728852(4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanoneAusbeute 99,9 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

A solution of 4-methyl-4-(pyrrolidine-1-carbonyl)piperidine-1-carboxylic acid tert-butyl ester (296 mg, 1.0 mmol) in TFA (5 mL), DCM (5 mL) and water (0.1 mL) was stirred at room temperature for 2 hours and then concentrated under reduced pressure. The residue was taken up in MeOH and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with MeOH and the desired product was eluted with 2M NH3 in MeOH. The solvents were removed to give the desired product as a white solid (196 mg, 66%). LCMS (Method A): RT 0.31 min; [M+H]+ 197

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. washThe cartridge was washed with MeOH
  3. washthe desired product was eluted with 2M NH3 in MeOH
  4. customThe solvents were removed

Quellen und Nachweise

ORD-Eintrag
ord-e9fa50f03ccb4474a83d7c8d5b11b311
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394796B2

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