Formic Acid → HCID 68991514, Verbindung

HRID 69497Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 69497
C(O[C:6](=O)[NH:7][C:8]1([CH3:20])[CH2:12][CH2:11][N:10]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:9]1)(C)(C)C.[OH-].[Na+].[CH:24](O)=O>>[CH2:13]([N:10]1[CH2:11][CH2:12][C:8]([N:7]([CH3:6])[CH3:24])([CH3:20])[CH2:9]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

Komponenten

4

Edukt 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 104937341,1-Dimethylethyl N-[3-methyl-1-(phenylmethyl)-3-pyrrolidinyl]carbamate

Produkt 1

HCID 68991514HCID 68991514, Verbindung

Versuchsvorschrift

A solution of (1-benzyl-3-methyl-pyrrolidin-3-yl)-carbamic acid tert-butyl ester (682 mg) in aqueous formic acid/aqueous formaldehyde 1:2 (7 mL) was stirred at 90° C. for 4 h. The mixture was neutralized with sodium hydroxide solution, extracted with dichloromethane, dried over magnesium sulfate and concentrated. The residue was purified by preparative HPLC. In this way the product was obtained with molecular weight 218.34 (C14H22N2); MS (ESI): 219 (M+H+).

Aufarbeitung

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by preparative HPLC
  5. customIn this way the product was obtained with molecular weight 218.34 (C14H22N2)

Quellen und Nachweise

ORD-Eintrag
ord-5b1cd6776485464fbdf6e7dd982762ed
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822495B2

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