Potassium Phosphate, Tribasic → Methyl 2-chloro-6-methanesulphonylamino-isonicotinate

HRID 74583

Reaktionsgleichung

Reaktionsgleichung von HRID 74583
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10](Cl)[N:11]=1)[C:5]([O:7][CH3:8])=[O:6].[CH3:13][S:14]([NH2:17])(=[O:16])=[O:15].P([O-])([O-])([O-])=O.[K+].[K+].[K+].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([NH:17][S:14]([CH3:13])(=[O:16])=[O:15])[N:11]=1)[C:5]([O:7][CH3:8])=[O:6]

Komponenten

7

Edukt 4

HCID 62657Potassium Phosphate, TribasicHCID 72879MethanesulfonamideHCID 93237Methyl 2,6-dichloroisonicotinateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)

Produkt 1

HCID 86615008Methyl 2-chloro-6-methanesulphonylamino-isonicotinate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere 10 g (49 mmol) methyl 2,6-dichloro-isonicotinate, 5.6 g (59 mmol) methanesulphonamide, 14 g (68 mmol) potassium phosphate, 1.7 g (2.9 mmol) Xantphos and 0.90 g tris(dibenzylideneacetone)dipalladium in 300 mL dioxane were stirred for 5 h at 100° C. The mixture was suction filtered through kieselguhr and evaporated down. The residue was stirred with ethanol and the solid was suction filtered.

Aufarbeitung

  1. filtrationfiltered through kieselguhr
  2. customevaporated down
  3. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-37bf25dc5c344be7a2563033c75a27d7
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829006B2

Verknüpfte Notizen

Wird geladen…