Calcium Carbonate → Methyl 2-(((methylamino)sulfonyl)amino)-3-pyridine carboxylate

HRID 66040

Reaktionsgleichung

Reaktionsgleichung von HRID 66040
[NH2:1][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[Ca+2].[CH3:17][NH:18][S:19](Cl)(=[O:21])=[O:20]>C(#N)C>[CH3:17][NH:18][S:19]([NH:1][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1)(=[O:21])=[O:20]

Komponenten

5

Edukt 3

HCID 10112Calcium CarbonateHCID 351633Methyl 2-aminopyridine-3-carboxylateHCID 11789235N-Methylsulfamoyl chloride

Produkt 1

HCID 22756775Methyl 2-(((methylamino)sulfonyl)amino)-3-pyridine carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Methyl 2-amino-3-pyridine carboxylate (15.2 grams; 0.1 mole), calcium carbonate (13.0 grams; 0.1 mole) and methylsulfamoyl chloride (13.0 grams; 0.1 mole) were mixed with 200 ml of acetonitrile and the resulting reaction mixture stirred at ambient temperatures for a period of about 15 hours. Following the reaction period, the reaction mixture was filtered and the solvent removed in vacuo. The semi-solid residue thus obtained was extracted with ethanol. A white crystalline precipitate, obtained by filtering the extract solution, was recrystallized from ethanol and the desired title compound having a melting point of 133° C.-139° C. was obtained.

Aufarbeitung

  1. customthe resulting reaction mixture
  2. customthe reaction period
  3. filtrationthe reaction mixture was filtered
  4. customthe solvent removed in vacuo
  5. customThe semi-solid residue thus obtained
  6. extractionwas extracted with ethanol
  7. customA white crystalline precipitate, obtained
  8. filtrationby filtering the extract solution
  9. customwas recrystallized from ethanol
  10. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-a825db44aa0a4164abb7535f1b9e3a48
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04129734

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