Potassium Carbonate → 2,5-dichloro-N-[4-(dimethylphosphoryl)phenyl]pyrimidin-4-amine

HRID 1471999Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1471999
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([Cl:9])=[CH:4][N:3]=1.[CH3:10][P:11]([C:14]1[CH:20]=[CH:19][C:17]([NH2:18])=[CH:16][CH:15]=1)([CH3:13])=[O:12].C(=O)([O-])[O-].[K+].[K+].C(=O)(O)[O-].[Na+]>CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:18][C:17]2[CH:16]=[CH:15][C:14]([P:11]([CH3:13])([CH3:10])=[O:12])=[CH:20][CH:19]=2)[C:5]([Cl:9])=[CH:4][N:3]=1

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 2372592,4,5-TrichloropyrimidineHCID 516892Sodium BicarbonateHCID 206345534-(Dimethylphosphoryl)aniline

Produkt 1

HCID 866687902,5-dichloro-N-[4-(dimethylphosphoryl)phenyl]pyrimidin-4-amineAusbeute 36,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

To a solution of 2,4,5-trichloropyrimidine (0.15 ml, 1.31 mmol) in 1 mL of DMF was added 4-(dimethylphosphoryl)aniline (0.221 g, 1.31 mmol) and potassium carbonate (0.217 g, 1.57 mmol). The mixture was heated at 110° C. for 4 h. It was basified with saturated sodium bicarbonate solution. The suspension was filtered and washed with ethyl acetate to give the final product (0.15 g, 36% yield). MS/ES+: m/z=316.

Aufarbeitung

  1. filtrationThe suspension was filtered
  2. washwashed with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c3670f113f034adbb1e27a2a3e1cda99
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09012462B2

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