Bromide ion → N,N,N',N'-Tetramethylbenzidine

HRID 329314

反応式

HRID 329314 の反応式
[CH3:1][N:2]([CH3:11])[C:3]1[CH:8]=[CH:7][C:6]([Mg]Br)=[CH:5][CH:4]=1.[Br-]>>[CH3:1][N:2]([CH3:11])[C:3]1[CH:8]=[CH:7][C:6]([C:6]2[CH:7]=[CH:8][C:3]([N:2]([CH3:11])[CH3:1])=[CH:4][CH:5]=2)=[CH:5][CH:4]=1

参加物

3

反応物 2

HCID 259Bromide ionHCID 178482849HCID 178482849、化合物

生成物 1

HCID 9702N,N,N',N'-Tetramethylbenzidine収率 70%

実験手順

A mixture of p-dimethylaminophenyl magnesium bromide (1 mole) and thallous bromide (2 moles) is stirred and refluxed under nitrogen for 5 hours. The cooled solution is filtered to remove thallium, and hydrogen chloride passed into the filtrate. The colorless hydrochloride which precipitates is filtered off, stirred into dilute sodium hydroxide, and the tetramethylbenzidine extracted with ether-benzene (1:1, 2 × 30 ml.) The extracts are dried over anhydrous sodium sulfate and the solvent removed to leave a yellow solid which is sublimed at 165°/0.05 mm. to give a 70% yield of pure N,N,N',N'-tetramethylbenzidine as a colorless solid, m.p. 195°.

後処理

  1. temperaturerefluxed under nitrogen for 5 hours
  2. filtrationThe cooled solution is filtered
  3. customto remove thallium, and hydrogen chloride
  4. customThe colorless hydrochloride which precipitates
  5. filtrationis filtered off
  6. extractionthe tetramethylbenzidine extracted with ether-benzene (1:1, 2 × 30 ml.) The extracts
  7. dry with materialare dried over anhydrous sodium sulfate
  8. customthe solvent removed
  9. customto leave a yellow solid which
  10. customis sublimed at 165°

出典と根拠

ORDレコード
ord-b0d7dbf2c85a46ec8aa432c160c0447e
出典データセット
uspto-grants-1977_04
特許番号
US04020073

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