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

HRID 465280ノート

反応式

HRID 465280 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7852223a462f4d96b9c43a3b7ce1ed21
出典データセット
uspto-grants-1992_10
特許番号
US05152824

反応ノート

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