StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Aniline → Pyrimido(5,4-d)pyrimidine

HRID 2238693
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2238693
Cl[C:2]1[N:3]=[C:4](Cl)[C:5]2[N:10]=[C:9](Cl)[N:8]=[C:7](Cl)[C:6]=2[N:13]=1.NC1C=CC=CC=1>C(Cl)(Cl)Cl>[N:10]1[C:5]2[CH:4]=[N:3][CH:2]=[N:13][C:6]=2[CH:7]=[N:8][CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6115AnilineHCID 97007Tetrachloropyrimido[5,4-d]pyrimidine

Produkt 1

HCID 21948654Pyrimido(5,4-d)pyrimidineAusbeute 199,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

In accord with the synthesis illustrated above, 4 g (19 mmol) of 2,4,6,8-tetrachloropyrimidopyrimidine was added to 50 ml of chloroform, and 8.7 ml (95 mmol) of aniline was slowly added in droplets thereto in a bath at 0° C. After the completion of the reaction was confirmed through TLC, the resulting reaction solution was washed with an aqueous ammonium chloride solution and then extracted with chloroform to separate an organic layer. Thereafter, the organic layer was distilled under reduced pressure to remove the solvent and then dried in an oven, yielding 5 g of a pale yellow solid 5a NMR analysis of the pale yellow solid produced the following data: 1H-NMR (DMSO-d6) d(ppm) 7.23 (t, 2H, J=7.3 z), 7.46 (t, 41, J=7.8 Hz), 7.87 (t, 4H, J=8.1 Hz), 8.66 (s, 2H).

Aufarbeitung

  1. additionwas slowly added in droplets
  2. customat 0° C
  3. customthe resulting reaction solution
  4. washwas washed with an aqueous ammonium chloride solution
  5. extractionextracted with chloroform
  6. customto separate an organic layer
  7. distillationThereafter, the organic layer was distilled under reduced pressure
  8. customto remove the solvent
  9. customdried in an oven

Quellen und Nachweise

ORD-Eintrag
ord-74c788c7f7894681b37456a3c06774c7
Quelldatensatz
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07719000B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion