N-bromobutanimide → 3-(Bromomethyl)-2,4-difluoro-1,1'-biphenyl

HRID 1995108ノート

反応式

HRID 1995108 の反応式
[F:1][C:2]1[C:7]([CH3:8])=[C:6]([F:9])[CH:5]=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Br:16]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:16][CH2:8][C:7]1[C:2]([F:1])=[C:3]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:4]=[CH:5][C:6]=1[F:9]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 128530332,4-Difluoro-3-methyl-1,1'-biphenyl

生成物 1

HCID 128530343-(Bromomethyl)-2,4-difluoro-1,1'-biphenyl収率 112.4%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A stirred solution of 2,4-difluoro-3-methyl[1,1'-biphenyl] (2.2 g, 0.011 mole) and N-bromosuccinimide (1.9 g, 0.011 mole) in 100 ml of carbon tetrachloride was irradiated with a 250 watt brooder lamp for 4 hours. The reaction mixture was allowed to reflux from the heat of the lamp. The reaction mixture was then filtered, and the filter cake was washed with three portions of carbon tetrachloride. The washes and filtrate were combined and evaporated under reduced pressure to give 3-bromomethyl-2,4-difluoro[1,1'-biphenyl] (3.5 g) as an oil whose nmr spectrum was consistent with that expected for the named compound.

後処理

  1. temperatureto reflux from the
  2. temperatureheat of the lamp
  3. filtrationThe reaction mixture was then filtered
  4. washthe filter cake was washed with three portions of carbon tetrachloride
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-49f836af65454c2aa770a7c7ffb6fe09
出典データセット
uspto-grants-1983_09
特許番号
US04402973

反応ノート

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