Sodium hydride → 4-Bromo-N,N-dimethyl-1H-imidazole-1-sulfonamide

HRID 1823966ノート

反応式

HRID 1823966 の反応式
[H-].[Na+].[Br:3][C:4]1[N:5]=[CH:6][NH:7][CH:8]=1.[CH3:9][N:10]([CH3:15])[S:11](Cl)(=[O:13])=[O:12]>O1CCCC1.[Cl-].[NH4+]>[CH3:9][N:10]([CH3:15])[S:11]([N:7]1[CH:8]=[C:4]([Br:3])[N:5]=[CH:6]1)(=[O:13])=[O:12]

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 83372Dimethylsulphamoyl chlorideHCID 178418934HCID 178418934、化合物

生成物 1

HCID 221479874-Bromo-N,N-dimethyl-1H-imidazole-1-sulfonamide収率 87%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 25517Ammonium Chloride溶媒

実験手順

Sodium hydride (55% in oil, 0.31 g) was added to a stirred solution of 4-bromo-1H imidazole (1.02 g) in dry tetrahydrofuran (20 mL) at room temperature under N2. After 10 minutes, dimethylsulfamoyl chloride (0.81 mL) was added. After stirring for 5 hours, the mixture was diluted with saturated aqueous ammonium chloride (20 mL) and extracted with ethyl acetate (20 mL). The extract was dried over Na2SO4, filtered and concentrated. The white solid was rinsed with diethyl ether and dried to give 1-(dimethylaminosulfonyl)-4-bromoimidazole (1.53 g, 87%). MS (ES+) 256, 254 ([MH]+).

後処理

  1. extractionextracted with ethyl acetate (20 mL)
  2. dry with materialThe extract was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washThe white solid was rinsed with diethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-f9432a21744c4234b7b4f2c364c7631c
出典データセット
uspto-grants-2006_05
特許番号
US07041689B2

反応ノート

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