Zinc Acetate → Zinc

HRID 373762

Reaktionsgleichung

Reaktionsgleichung von HRID 373762
[CH3:1][N:2]([C:16]1[CH:17]=[CH:18][C:19]([C:22]([NH:24][C@H:25]([C:31]([OH:33])=[O:32])[CH2:26][CH2:27][C:28]([OH:30])=[O:29])=[O:23])=[CH:20][CH:21]=1)[CH2:3][C:4]1[CH:5]=[N:6][C:7]2[N:13]=[C:12]([NH2:14])[N:11]=[C:10]([NH2:15])[C:8]=2[N:9]=1.C([O-])(=O)C.[Zn+2:38].C([O-])(=O)C>CO>[Zn:38].[CH3:1][N:2]([C:16]1[CH:17]=[CH:18][C:19]([C:22]([NH:24][C@H:25]([C:31]([OH:33])=[O:32])[CH2:26][CH2:27][C:28]([OH:30])=[O:29])=[O:23])=[CH:20][CH:21]=1)[CH2:3][C:4]1[CH:5]=[N:6][C:7]2[N:13]=[C:12]([NH2:14])[N:11]=[C:10]([NH2:15])[C:8]=2[N:9]=1

Komponenten

5

Edukt 2

HCID 11192Zinc AcetateHCID 126941Methotrexate2×

Produkt 2

HCID 23994ZincHCID 126941Methotrexate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

A zinc salt of methotrexate was prepared as follows. Methotrexate (3.0 g, 0.0066 moles) was dissolved in 600 ml methanol at room temperature with rapid stirring. A solution of zinc acetate (0.6 g, 0.0033 moles) in 2 ml methanol was added dropwise to the methotrexate solution. Immediate precipitation (flocculent) was observed. The mixture was stirred for one hour at room temperature. The mixture was then concentrated in a rotating evaporator (roto-vap) at 40° C. The residue obtained (3.2 g) was dried under high vacuum. (C20H22N8O5)2Zn, MW 974.29; percent zinc: 6.46 (found), 6.71 (theoretical).

Aufarbeitung

  1. customImmediate precipitation (flocculent)
  2. concentrationThe mixture was then concentrated in a rotating evaporator (roto-vap) at 40° C
  3. customThe residue obtained (3.2 g)
  4. customwas dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f0cda17369fe41d1bb7d8fe400482e47
Quelldatensatz
uspto-grants-1992_11
Patentnummer
US05166149

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