Dichloromethane → Ethylbis(2-chloroethyl)amine

HRID 472138

Reaktionsgleichung

Reaktionsgleichung von HRID 472138
S(Cl)([Cl:3])=O.[CH2:5]([N:7]([CH2:11]CO)[CH2:8][CH2:9]O)[CH3:6].C(=O)([O-])O.[Na+].Cl[CH2:20][Cl:21]>>[Cl:3][CH2:9][CH2:8][N:7]([CH2:11][CH2:20][Cl:21])[CH2:5][CH3:6]

Komponenten

5

Edukt 4

HCID 6344DichloromethaneHCID 8769EthyldiethanolamineHCID 24386Thionyl ChlorideHCID 516892Sodium Bicarbonate

Produkt 1

HCID 10848Ethylbis(2-chloroethyl)amineAusbeute 76 %

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

24 ml (330 mmol) of thionyl chloride are added dropwise to a solution of 20 g (150 mmol) of 2-[ethyl(2-hydroxyethyl)amino]ethanol in 200 ml of dichloromethane cooled beforehand to 0° C., and then the reaction medium is stirred at ambient temperature for 20 h. After the addition of a saturated aqueous solution of sodium hydrogen carbonate, the product is extracted with dichloromethane. The organic phase obtained is then washed with water, dried over magnesium sulfate, filtered and concentrated under vacuum. 19.5 g (76%) of bis(2-chloroethyl)ethylamine are obtained in the form of an oil.

Aufarbeitung

  1. extractionthe product is extracted with dichloromethane
  2. customThe organic phase obtained
  3. washis then washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-88e1ca256bec4b2abee104d9294a92db
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633196B2

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