p-Toluenesulfonic acid → HCID 178498584, Verbindung

HRID 1032582Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1032582
[OH:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][OH:12])[N:10]=[C:6]2[N:5]=[C:4]([C:13]([O:15][CH3:16])=[O:14])[CH:3]=1.CN(C=O)C.[C:22](OC(=O)C)(=[O:24])[CH3:23].C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[C:22]([O:12][CH2:11][C:9]1[N:10]=[C:6]2[N:5]=[C:4]([C:13]([O:15][CH3:16])=[O:14])[CH:3]=[C:2]([OH:1])[N:7]2[N:8]=1)(=[O:24])[CH3:23]

Komponenten

6

Edukt 4

HCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 178498586HCID 178498586, Verbindung

Produkt 1

HCID 178498584HCID 178498584, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of 25.7 g of 7-hydroxy-2-hydroxymethyl-5-methoxycarbonyl-s-triazolo[1,5-a]pyrimidine, 200 of DMF, 47 ml of acetic anhydride and 1 g of p-toluenesulfonic acid was stirred at 60° C. for 24 hours. The reaction mixture was condensed and 100 ml of methanol was added to the crystals precipitated residue, and the mixture was stirred. Then, crystals were collected by filtration, washed with methanol and dried to obtain 8.9 g of the title compound.

Aufarbeitung

  1. additionwas added to the crystals
  2. customprecipitated residue
  3. stirringthe mixture was stirred
  4. filtrationThen, crystals were collected by filtration
  5. washwashed with methanol
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-6ec77b0207f6434da0834788576b5971
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04958019

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