Trichloroacetic Acid → ASTA-Z-7654(free acid)

HRID 1651518Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1651518
[CH2:1]1[CH:7](O)[NH:6][P:4]([N:9]([CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][Cl:12])(=[O:5])[O:3][CH2:2]1.[CH:16]1([NH3+:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[SH:23][CH2:24][CH2:25][S:26]([O-:29])(=[O:28])=[O:27].ClC(Cl)(Cl)C(O)=O>O>[CH:16]1([NH3+:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[Cl:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][Cl:15])[P:4]1(=[O:5])[NH:6][CH:7]([S:23][CH2:24][CH2:25][S:26]([O-:29])(=[O:28])=[O:27])[CH2:1][CH2:2][O:3]1

Komponenten

5

Edukt 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 230498732-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1)

Produkt 1

HCID 6917796ASTA-Z-7654(free acid)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

5.6 g (20 mmol) of 4-hydroxycyclophosphamide (i.e., 2-(bis-(2-chloroethyl)-amino)-4-hydroxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide) and 4.8 g (20 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved in 100 ml of distilled water, mixed with some trichloroacetic acid and left to stand in a refrigerator for 3 days at 0° C. The solvent was then removed under high vacuum, the residue was taken up in acetone, re-concentrated, crystallised from acetone and recrystallised from isopropanol.

Aufarbeitung

  1. waitleft
  2. customThe solvent was then removed under high vacuum
  3. concentrationre-concentrated
  4. customcrystallised from acetone
  5. customrecrystallised from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-d8c2356f76a0498ba413e90956b162c2
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04929607

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