4-(3-Chloropropyl)morpholine → HCID 20303044, Verbindung

HRID 1732877Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1732877
[CH2:1]([N:3]([CH2:8][CH3:9])[C:4]([NH:6][CH3:7])=[O:5])[CH3:2].[Cl:10][CH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1>O1CCOCC1>[ClH:10].[CH2:1]([N:3]([CH2:8][CH3:9])[C:4]([N:6]([CH3:7])[CH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)=[O:5])[CH3:2]

Komponenten

4

Edukt 2

HCID 958344-(3-Chloropropyl)morpholineHCID 135031N,N-Diethyl-N'-methylurea

Produkt 1

HCID 20303044HCID 20303044, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

13 g (0.1 mole) of N,N-diethyl-N'methyl urea are dissolved in 100 cc. of anhydrous dioxane. 3.9 g (0.1 mole) of NaNH2 are added thereto and the reaction mixture is heated one hour at reflux. After cooling, 16.4 g (0.1 mole) of N-(3-chloropropyl)morpholine dissolved in 50 cc. of anhydrous dioxane are added thereto dropwise and the reaction mixture is refluxed for 6 hours. After cooling, the precipitated NaCl is filtered off with suction, the filtrate is evaporated and the remaining residue is subjected to fractionated distillation.

Aufarbeitung

  1. temperaturethe reaction mixture is heated one hour
  2. temperatureat reflux
  3. temperatureAfter cooling
  4. temperaturedropwise and the reaction mixture is refluxed for 6 hours
  5. temperatureAfter cooling
  6. filtrationthe precipitated NaCl is filtered off with suction
  7. customthe filtrate is evaporated
  8. distillationthe remaining residue is subjected to fractionated distillation

Quellen und Nachweise

ORD-Eintrag
ord-8bbe7d843dbb45bd82108f180c340889
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04239761

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