Formamidine acetate → HCID 178420898, Verbindung

HRID 1159174

Reaktionsgleichung

Reaktionsgleichung von HRID 1159174
[C:1]1([CH2:7][C@@H:8]([NH2:11])[CH2:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:12](O)(=O)C.C(N)=N>C(O)C>[CH2:7]([C@@H:8]1[CH2:9][NH:10][CH:12]=[N:11]1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 160693Formamidine acetateHCID 12699299(2R)-3-Phenylpropane-1,2-diamine

Produkt 1

HCID 178420898HCID 178420898, VerbindungAusbeute 93,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of (2R)-3-phenyl-1,2-propanediamine (0.20 g, 1.33 mmol) in ethanol (5 ml) was added formamidine acetate (0.15 g, 1.45 mmol) and the mixture was stirred overnight at room temperature. The solvent was evaporated, sodium hydroxide (2N, 5 ml) was added and the mixture was extracted 3 times with dichloromethane (10 ml). The combined organic layers were dried over magnesium sulfate and evaporated. The residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10) to yield a colorless oil (0.20 g, 92%); MS (ISP): 161.4 ((M+H)+).

Aufarbeitung

  1. customThe solvent was evaporated
  2. additionsodium hydroxide (2N, 5 ml) was added
  3. extractionthe mixture was extracted 3 times with dichloromethane (10 ml)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10)

Quellen und Nachweise

ORD-Eintrag
ord-0187ccd68ae8458c8f42c19f3058b348
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812047B2

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