N-bromobutanimide → 2-(Bromomethyl)-3-chloro-1,1'-biphenyl

HRID 485547

反応式

HRID 485547 の反応式
[Cl:1][C:2]1[C:3]([CH3:14])=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.[Br:15]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:15][CH2:14][C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=1[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 46018323-Chloro-2-methylbiphenyl

生成物 1

HCID 133207002-(Bromomethyl)-3-chloro-1,1'-biphenyl

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A stirred solution of 3-chloro-2-methyl-[1,1'-biphenyl] (13.5 g, 0.067 mole) and N-bromosuccinimide (11.8 g, 0.067 mole) in 125 ml of carbon tetrachloride was irradiated and heated to reflux for 61/2 hours with a 250 watt brooder lamp. The light/heat source was turned off and the reaction mixture stirred at room temperature for approximately 64 hours. The reaction mixture was again irradiated and heated for two hours with the brooder lamp. The mixture was cooled, a solid precipitate filtered off, and the filter cake washed with two 50 ml portions of carbon tetrachloride. The filtrate was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated under reduced pressure to give 2-bromomethyl-3-chloro-[1,1'-biphenyl] as an oil.

後処理

  1. temperatureheated
  2. temperatureto reflux for 61/2 hours with a 250 watt brooder lamp
  3. customThe reaction mixture was again irradiated
  4. temperatureheated for two hours with the brooder lamp
  5. temperatureThe mixture was cooled
  6. filtrationa solid precipitate filtered off
  7. washthe filter cake washed with two 50 ml portions of carbon tetrachloride
  8. washThe filtrate was washed with saturated aqueous sodium chloride solution
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-b7a18eff385e4042a9dc0af6f0add935
出典データセット
uspto-grants-1985_08
特許番号
US04536591

関連ノート

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