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

HRID 1065546노트

반응식

HRID 1065546 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f953b869395f4412af2a1a3adfba4b84
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04329518

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