Ici 109,081 → HCID 178430887, Verbindung

HRID 1088217

Reaktionsgleichung

Reaktionsgleichung von HRID 1088217
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]([CH3:15])[CH2:10][C:11](=[O:14])[NH:12][N:13]=2)=[CH:4][CH:3]=1.[CH3:16][C:17]1[C:18](=[O:24])[NH:19][C:20](=S)[NH:21][CH:22]=1>C(O)C>[CH3:16][C:17]1[C:18](=[O:24])[N:19]=[C:20]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:9]([CH3:15])[CH2:10][C:11](=[O:14])[NH:12][N:13]=3)=[CH:4][CH:3]=2)[NH:21][CH:22]=1

Komponenten

4

Edukt 2

HCID 161928Ici 109,081HCID 7204712-Thiothymine

Produkt 1

HCID 178430887HCID 178430887, VerbindungAusbeute 14,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

A stirred mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone (3.25 g) and 5-methylthiouracil (2.5 g) was heated at 180° C. for 11/2 hours. The residual gum was dissolved in hot aqueous ethanol and the solution was evaporated. Trituration of the residue with chloroform:methanol (10:1) gave the crude product as a solid (0.78 g), m.p. 260°-270° C. The filtrate was evaporated and the residue was heated at 180° C. for one hour. Purification of the residue by column chromatography (silica gel, chloroform:methanol, 25:1) gave a further amount of product (0.73 g).

Aufarbeitung

  1. customthe solution was evaporated
  2. customTrituration of the residue with chloroform:methanol (10:1) gave the crude product as a solid (0.78 g), m.p. 260°-270° C
  3. customThe filtrate was evaporated
  4. temperaturethe residue was heated at 180° C. for one hour
  5. customPurification of the residue by column chromatography (silica gel, chloroform:methanol, 25:1)

Quellen und Nachweise

ORD-Eintrag
ord-59fd5866dd4541f0b53485c68a1045d1
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04962110

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