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

HRID 66039

반응식

HRID 66039 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d751186db3c44b318877fb3211ccbabf
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129734

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