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

Dimethylformamide → 9-Phenyl-2-(3-pyridyl)purine-6-carboxamide

HRID 2427953
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2427953
[NH2:1][C:2]1[C:3]([C:21]([O:23]C)=O)=[N:4][C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[N:6]C=1NC1C=CC=CC=1.NC1C(C(OC)=O)=NC(Cl)=NC=1N[C:33]1[CH:38]=[CH:37]C=[CH:35][CH:34]=1.C([Sn](CCCC)(CCCC)C1C=[N:51]C=CC=1)CCC.[CH3:63][N:64]([CH:66]=O)[CH3:65]>>[C:65]1([N:64]2[CH:66]=[N:1][C:2]3[C:63]2=[N:6][C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[N:4][C:3]=3[C:21]([NH2:51])=[O:23])[CH:37]=[CH:38][CH:33]=[CH:34][CH:35]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 34838483-(Tributylstannyl)pyridineHCID 57474558Methyl 5-amino-2-chloro-6-(phenylamino)pyrimidine-4-carboxylateHCID 57474559Methyl 5-amino-6-(phenylamino)-2-(3-pyridyl)pyrimidine-4-carboxylate

Produkt 1

HCID 249378619-Phenyl-2-(3-pyridyl)purine-6-carboxamideAusbeute 57 %

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

Methyl 5-amino-6-(phenylamino)-2-(3-pyridyl)pyrimidine-4-carboxylate. To a solution of methyl 5-amino-2-chloro-6-(phenylamino)pyrimidine-4-carboxylate (0.189 g, 0.68 mmol) in anhydrous DMF (3.5 mL) was added 3-(tributylstannyl)pyridine (1.252 g, 3.4 mmol), and dichlorobis(triphenylphosphine) palladium(II) (0.239 g, 0.34 mmol). The solution was purged with nitrogen then heated in an Emrys Optimizer microwave reactor for 30 minutes at 120° C. The volatiles were evaporated and the resulting residue was purified using chromatography on a normal phase silica gel column (1-10% methanol in dichloromethane). Fractions containing product were combined and the solvent evaporated. The material was re-purified using reverse-phase preparatory HPLC (30-80% acetonitrile+0.1% TFA in H2O+0.1% TFA, over 30 minutes). Fractions containing the desired material were combined and concentrated under reduced pressure before being passed through a Strata-XC ion exchange column with water, methanol, and 5% ammonium hydroxide in methanol. The resulting solid was dried under high vacuum at 60° C. to afford the title compound (0.125 g, 0.389 mmol, 57% yield). MS (ESI) m/z 322.4 [M+1]+.

Aufarbeitung

  1. customThe solution was purged with nitrogen
  2. customThe volatiles were evaporated
  3. customthe resulting residue was purified
  4. additionFractions containing product
  5. customthe solvent evaporated
  6. customThe material was re-purified
  7. customreverse-phase preparatory HPLC (30-80% acetonitrile+0.1% TFA in H2O+0.1% TFA, over 30 minutes)
  8. additionFractions containing the desired material
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting solid was dried under high vacuum at 60° C.

Quellen und Nachweise

ORD-Eintrag
ord-d019e5f8a62b495694e8bfa0aa2e865f
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07968556B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion