Trichloroacetic Acid → 97139-59-8

HRID 2290841Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2290841
[CH2:1]([NH:8][C:9](=[O:12])[NH:10][OH:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC(Cl)(Cl)C(O)=O.[CH2:20]1[CH:26](O)[NH:25][P:23]([N:28]([CH2:32][CH2:33][Cl:34])[CH2:29][CH2:30][Cl:31])(=[O:24])[O:22][CH2:21]1>CC(C)=O.C(Cl)Cl>[CH2:1]([NH:8][C:9](=[O:12])[N:10]([OH:11])[CH:26]1[CH2:20][CH2:21][O:22][P:23]([N:28]([CH2:32][CH2:33][Cl:34])[CH2:29][CH2:30][Cl:31])(=[O:24])[NH:25]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 13770898N-Benzyl-N'-hydroxyurea

Produkt 1

HCID 1377089997139-59-8

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

540 mg (3.25 mmol) of 3-benzyl-1-hydroxyurea in 40 ml of acetone and a catalytic amount of trichloroacetic acid were added to 900 mg (3.25 mmol) of 4-hydroxycyclophosphamide in 1 ml of methylenechloride. The mixture was stored overnight at -25° C., the crystals were then drawn off by suction, washed with acetone and ether and recrystallized from ethyl acetate.

Aufarbeitung

  1. washwashed with acetone and ether
  2. customrecrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-98245b4734e949f4abb48ec7ade04ca1
Quelldatensatz
uspto-grants-1986_10
Patentnummer
US04618692

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