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

HRID 1651519

Reaktionsgleichung

Reaktionsgleichung von HRID 1651519
[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>CO>[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 887MethanolLösungsmittel

Versuchsvorschrift

1.4 g (5 mmol) of 4-hydroxycyclophosphamide and 1.2 g (5 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved together with a trace of trichloroacetic acid in 25 ml of methanol and were left to stand overnight in a refrigerator at -25° C. The reaction solution was then concentrated to about 5 ml, ether was added until clouding commensed and the mixture was triturated. The crystallised material was filtered with suction after standing for 20 hours at 0° C., and was washed and dried.

Aufarbeitung

  1. waitwere left
  2. concentrationThe reaction solution was then concentrated to about 5 ml, ether
  3. additionwas added
  4. customthe mixture was triturated
  5. filtrationThe crystallised material was filtered with suction
  6. waitafter standing for 20 hours at 0° C.
  7. washwas washed
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7e10a76758044ff2a956a538a9019d42
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04929607

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