Sodium Carbonate → HCID 178488969, Verbindung

HRID 235970Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 235970
[C:1]([C:4]1[N:5]=[C:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[NH:7][CH:8]=1)(=O)[NH2:2].C([O-])([O-])=O.[Na+].[Na+]>O=P(Cl)(Cl)Cl>[C:1]([C:4]1[N:5]=[C:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[NH:7][CH:8]=1)#[N:2]

Komponenten

4

Edukt 2

HCID 10340Sodium CarbonateHCID 178488972HCID 178488972, Verbindung

Produkt 1

HCID 178488969HCID 178488969, VerbindungAusbeute 71,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

A mixture of 64 (7.6 g, 0.035 mol) and POCl3 (100 ml) was heated at reflux for 5.5 hours. After stirring at room temperature overnight, the suspension was poured into saturated Na2CO3 and the mixture extracted with 20% CH3OH--CHCl3 (3×). The organic extracts were washed with saturated NaCl, dried, filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product eluted with 5% CH3OH--CHCl3 to yield 5.0 g (71%) of 65; m.p. 219°-20° C. (CH3CN).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 5.5 hours
  3. extractionthe mixture extracted with 20% CH3OH
  4. washThe organic extracts were washed with saturated NaCl
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. customThe residue was chromatographed on silica gel
  9. washthe product eluted with 5% CH3OH

Quellen und Nachweise

ORD-Eintrag
ord-db0d841ebcff40da8b8d546fb8cf9489
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04642311

Notizen zur Reaktion

Wird geladen…