Triethylamine → Cyclophosphamide

HRID 659310

Reaktionsgleichung

Reaktionsgleichung von HRID 659310
[Cl:1][CH2:2][CH2:3][N:4]([CH2:9][CH2:10][Cl:11])[P:5](Cl)(Cl)=[O:6].CN[C:14]([C:18]1[CH:23]=CC=CC=1)([OH:17])CC.C([N:26](CC)CC)C>C(OCC)(=O)C>[CH2:18]1[CH2:14][O:17][P:5]([N:4]([CH2:9][CH2:10][Cl:11])[CH2:3][CH2:2][Cl:1])(=[O:6])[NH:26][CH2:23]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 96271Phosphoramidic dichloride, bis(2-chloroethyl)-HCID 19933884HCID 19933884, Verbindung

Produkt 1

HCID 2907Cyclophosphamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A solution of bis(2-chloroethyl)phosphoramidic dichloride (10 mmol) in ethyl acetate (100 mL) is added dropwise to a solution of commercial 3 methylamino-1-phenyl-1-propanol (10 mmol) and triethylamine (20 mmol) in ethyl acetate (100 mL) at rt. After stirring at rt for 3 days, the salts are filtered off and the combined filtrates are concentrated under vacuum. The crude product is purified by column chromatography on silica.

Aufarbeitung

  1. filtrationthe salts are filtered off
  2. concentrationthe combined filtrates are concentrated under vacuum
  3. customThe crude product is purified by column chromatography on silica

Quellen und Nachweise

ORD-Eintrag
ord-ba24910390c54d239897abdfb963ae7b
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08080536B2

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