Carbonic acid-guanidine (1:1) → Aditeren

HRID 414526

Reaktionsgleichung

Reaktionsgleichung von HRID 414526
[Na].C(=O)(O)O.[NH2:6][C:7]([NH2:9])=[NH:8].[NH:10]([CH:17]=[C:18]([C:33]#N)[CH2:19][C:20]1[CH:28]=[C:27]([O:29][CH3:30])[C:23]([NH:24]C=O)=[C:22]([O:31][CH3:32])[CH:21]=1)C1C=CC=CC=1>O>[NH2:8][C:7]1[N:9]=[C:17]([NH2:10])[C:18]([CH2:19][C:20]2[CH:21]=[C:22]([O:31][CH3:32])[C:23]([NH2:24])=[C:27]([O:29][CH3:30])[CH:28]=2)=[CH:33][N:6]=1

Komponenten

5

Edukt 3

HCID 286947Carbonic acid-guanidine (1:1)HCID 5360545SodiumHCID 867400924'-(3-Anilino-2-cyano-allyl)-2',6'-dimethoxy-formanilide

Produkt 1

HCID 176875Aditeren

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 1.84 g. of sodium in 200 ml. of absolute alcohol was treated with 14.4 g. guanidine carbonate and 8.9 g. of 4'-(3-anilino-2-cyano-allyl)-2',6'-dimethoxy-formanilide and refluxed for 20 hours. Then, 200 ml. of water were added and the alcohol was removed under vacuum. After standing at room temperature for 2 hours, the crystals formed were removed by filtration with suction, washed with water and recrystallized from methanol, whereby there was obtained 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-pyrimidine having a melting point of 215°-216° C.

Aufarbeitung

  1. customthe alcohol was removed under vacuum
  2. customthe crystals formed
  3. customwere removed by filtration with suction
  4. washwashed with water
  5. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-023acfce3a31477593b23bb8fe5cc290
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04792557

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