Reaktion #94193

ord-236fd08383f64e2cb363e09d99783ced

Reaktionsgleichung

Cn1c(NO)cc(=O)n(C)c1=O
1,3-dimethyl-6-hydroxyaminouracil
CCOC([O-])[O-]
ethyl orthoformate
→
Cn1c(=O)c2conc2n(C)c1=O
captioned compound
Cn1c(=O)c2conc2n(C)c1=O
5,7-Dimethyl-5H,7H-isoxazolo[3,4-d]pyrimidine-4,6-dione

Edukte

Cn1c(NO)cc(=O)n(C)c1=O
1,3-dimethyl-6-hydroxyaminouracil
CCOC([O-])[O-]
ethyl orthoformate

Reagenzien

Keine

Lösungsmittel

CN(C)C=O
dimethylformamide

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefor 1 hour
  2. 2
    workup.DISTILLATIONafter which the solvent is distilled off
  3. 3
    workup.ADDITIONTo the residue is added ethanol
  4. 4
    Filtrationthe resultant crystals are collected by filtration
  5. 5
    SonstigeAs recrystallized from hot water

Vorschrift

A mixture of 2 g of 1,3-dimethyl-6-hydroxyaminouracil, 20 ml of dimethylformamide and 20 ml of ethyl orthoformate is boiled at 160° C. for 1 hour, after which the solvent is distilled off. To the residue is added ethanol and the resultant crystals are collected by filtration. As recrystallized from hot water, 1.0 g of the captioned compound is obtained as colorless prisms, melting point: 170°-171° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04129654uspto-grants-1978_12