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N,N'-Dimethylethylenediamine → 3-bromo-N-(2-(dimethylamino)ethyl)benzenesulfonamide

HRID 238350
ノート
印刷プレビュー

反応式

HRID 238350 の反応式
C[NH:2][CH2:3][CH2:4][NH:5][CH3:6].[CH2:7](N(CC)CC)C.[Br:14][C:15]1[CH:16]=[C:17]([S:21](Cl)(=[O:23])=[O:22])[CH:18]=[CH:19][CH:20]=1>C(Cl)(Cl)Cl>[Br:14][C:15]1[CH:16]=[C:17]([S:21]([NH:2][CH2:3][CH2:4][N:5]([CH3:6])[CH3:7])(=[O:23])=[O:22])[CH:18]=[CH:19][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8070N,N'-DimethylethylenediamineHCID 8471TriethylamineHCID 17943m-Bromobenzenesulphonyl chloride

生成物 1

HCID 38617893-bromo-N-(2-(dimethylamino)ethyl)benzenesulfonamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Under cooling in an ice bath, N,N′-dimethylethylenediamine (414 mg) and triethylamine (1.10 mL) were added to a chloroform (10 mL) solution of 3-bromobenzenesulfonyl chloride (1.00 g), and the obtained solution was then stirred at a room temperature for 45 minutes. The reaction solution was washed with water, and was then dried over anhydrous sodium sulfate, followed by vacuum concentration. The residue was purified by column chromatography (silica gel 60N, chloroform:methanol=98:2 to 96:4), so as to obtain the title compound (1.14 g) in the form of a colorless solid.

後処理

  1. temperatureUnder cooling in an ice bath
  2. washThe reaction solution was washed with water
  3. dry with materialwas then dried over anhydrous sodium sulfate
  4. concentrationfollowed by vacuum concentration
  5. customThe residue was purified by column chromatography (silica gel 60N, chloroform:methanol=98:2 to 96:4)

出典と根拠

ORDレコード
ord-f01e4ddc901c4d7b840da4fc1fa1f0c5
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642626B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート