Triethylamine → N,N-dimethyl-4-[2-methyl-2-(trifluoromethyl)but-3-en-1-yl]-1H-imidazole-1-sulfonamide

HRID 425325ノート

反応式

HRID 425325 の反応式
C(N(CC)CC)C.[CH3:8][N:9]([CH3:14])[S:10](Cl)(=[O:12])=[O:11].[CH3:15][C:16]([C:25]([F:28])([F:27])[F:26])([CH:23]=[CH2:24])[CH2:17][C:18]1[N:19]=[CH:20][NH:21][CH:22]=1>C(Cl)Cl.O>[CH3:8][N:9]([CH3:14])[S:10]([N:21]1[CH:22]=[C:18]([CH2:17][C:16]([CH3:15])([C:25]([F:26])([F:27])[F:28])[CH:23]=[CH2:24])[N:19]=[CH:20]1)(=[O:12])=[O:11]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 83372Dimethylsulphamoyl chlorideHCID 178442249HCID 178442249、化合物

生成物 1

HCID 59140382N,N-dimethyl-4-[2-methyl-2-(trifluoromethyl)but-3-en-1-yl]-1H-imidazole-1-sulfonamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (3 mL, 14.02 mmol) followed by dimethylsulfamoyl chloride (1.5 mL, 14.02 mmol) were added to an ambient temperature solution of 4-[2-methyl-2-(trifluoromethyl)but-3-en-1-yl]-1H-imidazole (1.43 g, 7.01 mmol) in methylene chloride (20 mL). After stirring at ambient temperature overnight, the reaction mixture was diluted with water and extracted with ethyl acetate and methylene chloride. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-100% ethyl acetate/hexane afforded the title compound.

後処理

  1. extractionextracted with ethyl acetate and methylene chloride
  2. dry with materialThe combined organic extracts were dried (magnesium sulfate)
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-865bcd1cd2ec4e8b849919ca407b8b51
出典データセット
uspto-grants-2012_01
特許番号
US08106070B2

反応ノート

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