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Propylamine → N-Butyl-N'-propylurea

HRID 2248418
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2248418
[CH2:1]([NH2:4])[CH2:2][CH3:3].[CH2:5]([N:9]=[C:10]=[O:11])[CH2:6][CH2:7][CH3:8]>ClCCl>[CH2:1]([NH:4][C:10]([NH:9][CH2:5][CH2:6][CH2:7][CH3:8])=[O:11])[CH2:2][CH3:3]
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Komponenten

4

Edukt 2

HCID 7852PropylamineHCID 8110Butyl isocyanate

Produkt 1

HCID 14836212N-Butyl-N'-propylureaAusbeute 92,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

205.8 Grams (3.48 moles) of n-propylamine and 250 ml of dichloromethane were charged to a round bottom flask equipped with stirrer, thermometer, reflux condenser and dropping funnel. 313.7 Grams (3.16 moles) of butyl isocyanate were added to the dropping funnel and then metered into the flask with stirring and strong external cooling (solid CO2 bath) at a rate slow enough to maintain the contents generally below 0° C. except for brief excursions to higher temperatures. The resulting mixture was left to stand overnight and then freed of solvent and lights under vacuum with a rotary evaporator leaving 462.3 g of crude product (92.6% crude yield). After further drying of a portion under vacuum a 97.6 area % purity was recorded by gas chromatography. The product contained substantially only one compound by gas chromatography. It melted at 70°-72° C.

Aufarbeitung

  1. customequipped with stirrer
  2. temperaturethermometer, reflux condenser
  3. temperaturestrong external cooling (solid CO2 bath) at a rate slow enough
  4. temperatureto maintain the contents generally below 0° C. except for brief excursions to higher temperatures
  5. waitThe resulting mixture was left
  6. customfreed of solvent and lights under vacuum with a rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-85e328f7d80c40549910ddbf25c1d694
Quelldatensatz
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05039759

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