Sulfuric acid magnesium salt (1:1) → HCID 23446882, Verbindung

HRID 1841634Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1841634
[NH2:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([CH3:11])[C:3]=1[C:4]#[N:5].[CH3:12][C:13]1[N:18]=[C:17]2[C:19]([O:21][C:22](=O)[C:16]2=[CH:15][CH:14]=1)=[O:20].S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[Cl:10][C:9]1[C:2]([N:1]2[C:22](=[O:21])[C:16]3[C:17](=[N:18][C:13]([CH3:12])=[CH:14][CH:15]=3)[C:19]2=[O:20])=[C:3]([C:4]#[N:5])[C:6]([CH3:11])=[CH:7][CH:8]=1

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 13345321HCID 13345321, VerbindungHCID 23446892HCID 23446892, Verbindung

Produkt 1

HCID 23446882HCID 23446882, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
170 °C

Versuchsvorschrift

3.1 g (18.61 mmol) of the compound from example 4 were added to 2.9 g (17.7 mmol) of 6-methylpyridine-2,3-dicarboxylic anhydride and, with warming to 170° C., the mixture was stirred for a total of 8 h as a melt. After cooling, the residue was taken up in methylene chloride, and the solution was treated with active carbon and magnesium sulfate. After filtering off with suction, the filtrate was chromatographed on silica gel, 1.3 g (24.4% of theory) of the title compound being obtained after concentration as beige crystals of m.p. 173-176° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationAfter filtering off with suction
  3. customthe filtrate was chromatographed on silica gel, 1.3 g (24.4% of theory) of the title compound
  4. custombeing obtained
  5. concentrationafter concentration as beige crystals of m.p. 173-176° C.

Quellen und Nachweise

ORD-Eintrag
ord-3d4e2b211cc54807b9cf22ee1050d50c
Quelldatensatz
uspto-grants-2004_01
Patentnummer
US06683213B1

Notizen zur Reaktion

Wird geladen…