Isopropylsulphamoyl chloride → Methyl 2-((((1-methylethyl)amino)sulfonyl)amino)-3-pyridine carboxylate

HRID 65815

反応式

HRID 65815 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.[CH:12]([NH:15][S:16](Cl)(=[O:18])=[O:17])([CH3:14])[CH3:13]>C1C=CC=CC=1>[CH3:13][CH:12]([NH:15][S:16]([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:18])=[O:17])[CH3:14]

参加物

4

反応物 2

HCID 117737Isopropylsulphamoyl chlorideHCID 351633Methyl 2-aminopyridine-3-carboxylate

生成物 1

HCID 13609242Methyl 2-((((1-methylethyl)amino)sulfonyl)amino)-3-pyridine carboxylate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Methyl 2-amino-3-pyridine carboxylate (10.0 grams; 0.066 mole) and isopropyl sulfamoyl chloride (11.4 grams; 0.066 mole) were mixed with 300 ml of benzene and the resulting reaction mixture heated at reflux temperatures for a period of 48 hours. Following the reaction period, the reaction mixture was cooled and the solvent removed in vacuo. The oily residue thus obtained was extracted with 200 ml of cyclohexane and the extracts combined and cooled. The resulting precipitate was recovered by filtration and recrystallized from carbon tetrachloride. As a result of these operations, the desired title compound having a melting point of 121° C.-123° C. was obtained.

後処理

  1. customthe resulting reaction mixture
  2. temperatureheated
  3. temperatureat reflux temperatures for a period of 48 hours
  4. customthe reaction period
  5. temperaturethe reaction mixture was cooled
  6. customthe solvent removed in vacuo
  7. customThe oily residue thus obtained
  8. extractionwas extracted with 200 ml of cyclohexane
  9. temperaturecooled
  10. filtrationThe resulting precipitate was recovered by filtration
  11. customrecrystallized from carbon tetrachloride
  12. customAs a result of these operations

出典と根拠

ORDレコード
ord-ccb6f5638f4a4496b803c0011606f82f
出典データセット
uspto-grants-1978_12
特許番号
US04128551

関連ノート

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