phenyl N-[(N-dimethylsulfamoyl-N-methylamino)sulfonyl]carbamate → 1-[(N-dimethylsulfamoyl-N-methylamino)sulfonylcarbamoyl]-3-methyl-5-(2-thienyl)-2-pyrazoline

HRID 465280노트

반응식

HRID 465280 반응식
[CH3:1][N:2]([CH3:21])[S:3]([N:6]([S:8]([NH:11][C:12](=[O:20])OC1C=CC=CC=1)(=[O:10])=[O:9])[CH3:7])(=[O:5])=[O:4].[CH3:22][C:23]1[CH2:27][CH:26]([C:28]2[S:29][CH:30]=[CH:31][CH:32]=2)[NH:25][N:24]=1>C1C=CC=CC=1>[CH3:21][N:2]([CH3:1])[S:3]([N:6]([S:8]([NH:11][C:12]([N:25]1[CH:26]([C:28]2[S:29][CH:30]=[CH:31][CH:32]=2)[CH2:27][C:23]([CH3:22])=[N:24]1)=[O:20])(=[O:9])=[O:10])[CH3:7])(=[O:4])=[O:5]

참가 물질

4

반응물 2

HCID 19873528phenyl N-[(N-dimethylsulfamoyl-N-methylamino)sulfonyl]carbamateHCID 198735293-Methyl-5-(2-thienyl)-2-pyrazoline

생성물 1

HCID 198735301-[(N-dimethylsulfamoyl-N-methylamino)sulfonylcarbamoyl]-3-methyl-5-(2-thienyl)-2-pyrazoline수율 76.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture comprising 1.69 g (5.0 mmol) of phenyl N-[(N-dimethylsulfamoyl-N-methylamino)sulfonyl]carbamate, 0.58 g (3.5 mmol) of 3-methyl-5-(2-thienyl)-2-pyrazoline and 10 ml of dry benzene, was refluxed for 10 minutes. The mixture was left to cool, and then benzene was distilled off under reduced pressure. The obtained residue was washed with n-hexane. Then, the residue was stirred together with diethyl ether. The precipitated crystalline product was isolated by suction filtration and then washed with diethyl ether to obtain 1.1 g of the desired 1-[(N-dimethylsulfamoyl-N-methylamino)sulfonylcarbamoyl]-3-methyl-5-(2-thienyl)-2-pyrazoline.

후처리

  1. waitThe mixture was left
  2. temperatureto cool
  3. distillationbenzene was distilled off under reduced pressure
  4. washThe obtained residue was washed with n-hexane
  5. customThe precipitated crystalline product was isolated by suction filtration
  6. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-7852223a462f4d96b9c43a3b7ce1ed21
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05152824

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