Formaldehyde → HCID 19600111, Verbindung

HRID 611240Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 611240
[CH2:1]([NH:8][CH2:9][CH2:10][C:11]1[CH:15]=[CH:14][O:13][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]=O>C(O)(=O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11]2[CH:15]=[CH:14][O:13][C:12]=2[CH2:16]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 712FormaldehydeHCID 19600250HCID 19600250, Verbindung

Produkt 1

HCID 19600111HCID 19600111, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of 5.603 g (27.838 mmol) of N-benzyl-2-(3-furyl)ethylamine in 50 ml of acetic acid, 2.71 g (33.4 mmol) of 37% aqueous formaldehyde was added, followed by stirring at 100° C. for 1 hour. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1) to yield the desired product.

Aufarbeitung

  1. distillationAfter the solvent was distilled off under reduced pressure
  2. extractionextracted with dichloromethane 3 times
  3. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1)

Quellen und Nachweise

ORD-Eintrag
ord-5fbee235727342598dcf324d0864cc4c
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US05998433

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