Formaldehyde → HCID 178481284, Verbindung

HRID 1682657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1682657
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([OH:8])[CH2:4][CH2:3]1.[CH3:9][N:10](C)[C:11](N)=O.C=[O:16].[CH3:17][N:18]1[CH2:23]COC[CH2:19]1>C1(C)C=CC=CC=1.O1CCOCC1>[OH:8][C@H:5]1[CH2:6][CH2:7][C@H:2]([N:1]2[CH2:9][N:10]([CH3:11])[C:23](=[O:16])[N:18]([CH3:17])[CH2:19]2)[CH2:3][CH2:4]1

Komponenten

7

Edukt 4

HCID 712FormaldehydeHCID 79724-MethylmorpholineHCID 11737N,N-DimethylureaHCID 178511715HCID 178511715, Verbindung

Produkt 1

HCID 178481284HCID 178481284, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a mixture of trans-4-aminocyclohexanol (5.00 g, 43.4 mmol), N,N-dimethylurea (3.82 g, 43.4 mmol), 37% formalin (50 ml), N-methylmorpholine (9.54 ml, 86.8 mmol) and dioxane (10 ml) was added toluene (200 ml), and the mixture was heated for about 5 hours while removing water for azeotropic distillation. Low boiling matters were distilled away from the reaction mixture under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/methanol=50/1-10/1) to give 7.40 g of trans-5-(4-hydroxycyclohexyl)-1,3-dimethylhexahydro-2-oxo-1,3,5-triazine as colorless solid (75%).

Aufarbeitung

  1. temperaturethe mixture was heated for about 5 hours
  2. customwhile removing water
  3. distillationfor azeotropic distillation
  4. distillationwere distilled away from the reaction mixture under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=50/1-10/1)

Quellen und Nachweise

ORD-Eintrag
ord-94052f69a8c84488a203e09dd5e50335
Quelldatensatz
uspto-grants-1997_06
Patentnummer
US05635527

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