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

HRID 992851Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 992851
[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 A4 were added to 2.9 g (17.7 mmol) of 6-methylpyridine-2,3-dicarboxylic anhydride and, after heating to 170° C., stirred as a melt for a total of 8 h. After cooling, the residue was taken up in methylene chloride, and activated carbon and magnesium sulfate were added. The mixture was filtered off with suction and chromatographed on silica gel giving, after concentration, 1.3 g (24.4% of theory) of the title compound as beige crystals of m.p. 173-176° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationThe mixture was filtered off with suction
  3. customchromatographed on silica gel giving
  4. concentrationafter concentration, 1.3 g (24.4% of theory) of the title compound as beige crystals of m.p. 173-176° C.

Quellen und Nachweise

ORD-Eintrag
ord-18a3936b51644059b060c008179a7973
Quelldatensatz
uspto-grants-2002_10
Patentnummer
US06472349B1

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