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

HRID 66045

反応式

HRID 66045 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4a0ffd53325a46408ed2bf42b18c23d4
出典データセット
uspto-grants-1978_12
特許番号
US04129733

関連ノート

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