Water → Aditeren

HRID 462526

Reaktionsgleichung

Reaktionsgleichung von HRID 462526
O.[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([NH2:19])=[C:13]([O:20][CH3:21])[CH:12]=2)=[C:5](Cl)[N:4]=1>[Hg](Cl)Cl.[Zn].C(O)(=O)C>[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:12]=[C:13]([O:20][CH3:21])[C:14]([NH2:19])=[C:15]([O:17][CH3:18])[CH:16]=2)=[CH:5][N:4]=1

Komponenten

6

Edukt 2

HCID 962WaterHCID 21280993HCID 21280993, Verbindung

Produkt 1

HCID 176875Aditeren

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23994ZincKatalysatorHCID 24085Mercuric ChlorideKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of 0.1 g. of mercury (II) chloride in 2 ml. of water and 1.5 g. of zinc powder was added to a solution of 1.5 g. of 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-6-chloropyrimidine in 15.5 ml. of glacial acetic acid and the mixture was boiled under reflux with stirring overnight. Then, the mixture was filtered while hot and the zinc powder washed with 5 ml. of acetic acid. The combined filtrates were added dropwise with stirring at a temperature below 20° C. to 40 ml. of concentrated ammonia. Then, the mixture was stirred at 20° C. for an additional hour and the solid material was removed by filtration under vacuum, washed with water, dried, recrystallized from methanol and there was obtained 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-pyrimidine having a melting point of 214° C.

Aufarbeitung

  1. temperatureunder reflux
  2. filtrationThen, the mixture was filtered while hot and the zinc powder
  3. washwashed with 5 ml
  4. additionThe combined filtrates were added dropwise
  5. stirringwith stirring at a temperature below 20° C. to 40 ml
  6. stirringThen, the mixture was stirred at 20° C. for an additional hour
  7. customthe solid material was removed by filtration under vacuum
  8. washwashed with water
  9. customdried
  10. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-299ac4868f0c4bd7a5ae90f14d411515
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04515948

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