Stannous chloride dihydrate → HCID 10967548, Verbindung

HRID 377500Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 377500
[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)[C:9]([N+:17]([O-])=O)=[C:8]([CH:20]([CH3:22])[CH3:21])[N:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.O.O.[Sn](Cl)Cl>C(O)C>[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)[C:9]([NH2:17])=[C:8]([CH:20]([CH3:22])[CH3:21])[N:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

Komponenten

4

Edukt 2

HCID 61436Stannous chloride dihydrateHCID 53792902HCID 53792902, Verbindung

Produkt 1

HCID 10967548HCID 10967548, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Dissolve 2,4-bis(1H-imidazol-1-yl)-5-nitro-6-(2-propyl)pyrimidine (16 g, 53.5 mmol) in 300 mL of ethanol and add 35 g of tin (II) chloride dihydrate. Stir for 2 hours at ambient temperature. Remove the solvent under vacuum and slurry the residue in 2 L of CH2Cl2. Wash with 2×3 L 10% KOH. Dry the CH2Cl2 portion over MgSO4, treat with charcoal, filter, and concentrate the filtrate under vacuum. Crystallize the residue from ethyl acetate to provide 2,4-bis(1H-imidazol-1-yl)-6-(2-propyl)pyrimidin-5-amine.

Aufarbeitung

  1. customRemove the solvent under vacuum
  2. washWash with 2×3 L 10% KOH
  3. dry with materialDry the CH2Cl2 portion over MgSO4
  4. additiontreat with charcoal
  5. filtrationfilter
  6. concentrationconcentrate the filtrate under vacuum
  7. customCrystallize the residue from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c14fb4bc005b4880828a8b1c25e04c88
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06025489

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