4-Methylmorpholine → Cyclophosphamide

HRID 518591

Reaktionsgleichung

Reaktionsgleichung von HRID 518591
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].CN1CCOCC1.[O:13]=[P:14](Cl)(Cl)Cl.Cl.[Cl:19][CH2:20][CH2:21][NH:22][CH2:23][CH2:24][Cl:25]>>[CH2:3]1[CH2:4][O:5][P:14]([N:22]([CH2:23][CH2:24][Cl:25])[CH2:21][CH2:20][Cl:19])(=[O:13])[NH:1][CH2:2]1

Komponenten

5

Edukt 4

HCID 79724-MethylmorpholineHCID 90863-Amino-1-propanolHCID 24813Phosphorus oxychloride2×HCID 522769Bis(2-chloroethyl)amine hydrochloride

Produkt 1

HCID 2907Cyclophosphamide

Versuchsvorschrift

3-aminopropanol (2.1 g, 0.028 mol) and N-methylmorpholine (12.9 eq) are placed into a three-necked flask and stirred at room temperature. After cooling the mixture in the flask, POCl3 (4.3 g, 0.028 mol) is slowly dropped into the mixture. After adding POCl3, the mixture in the flask is stirred at room temperature for 15 hours. After that, bis(2-chloroethyl)amine hydrochloride] (5 g, 0.028 mol) is added into the mixture in the flask. The mixture in the flask is heated to about 40° C. and stirred for 6 hours. (The conversion yield determined with HPLC is about 10.0%.)

Aufarbeitung

  1. additionis slowly dropped into the mixture
  2. stirringthe mixture in the flask is stirred at room temperature for 15 hours
  3. temperatureThe mixture in the flask is heated to about 40° C.
  4. stirringstirred for 6 hours
  5. custom(The conversion yield

Quellen und Nachweise

ORD-Eintrag
ord-476edc016270404d86d4aa37bb45a02b
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09115160B2

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