Diisopropylamine → 1-Bromo-3-chloro-2,4-difluorobenzene

HRID 1699997

反応式

HRID 1699997 の反応式
C(NC(C)C)(C)C.[F:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[Br:16].[Cl:17]C(Cl)(Cl)C(C(Cl)(Cl)Cl)=O>C([Li])CCC>[Cl:17][C:14]1[C:9]([F:8])=[C:10]([Br:16])[CH:11]=[CH:12][C:13]=1[F:15]

参加物

5

反応物 3

HCID 7912DiisopropylamineHCID 8303HexachloroacetoneHCID 676741-Bromo-2,4-difluorobenzene

生成物 1

HCID 27732561-Bromo-3-chloro-2,4-difluorobenzene

試薬・触媒・溶媒 1

HCID 178418339Butyllithium溶媒

反応条件

温度
0 °C

実験手順

To a solution of 19 ml (0.135 mole) of diisopropylarnine in 125 ml of tetrahydroflran (TBF) cooled at −20° C. is added 80 ml of n-butyllithium (1.6 M in hexane). The temperature is raised to 0° C. for 5 minutes and lowered to −78° C. Then 25 g (0.129 mole) of 2,4-difluoro-bromobenzene is then added and the reaction is stirred at −65° C. for 2 hours. Then, 25 ml (0.164 mole) of hexachloroacetone is added and the solution is warmed at room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.

後処理

  1. customlowered to −78° C
  2. temperaturethe solution is warmed at room temperature
  3. customAfter evaporation of the solvent
  4. distillationthe residue is distilled under vacuum

出典と根拠

ORDレコード
ord-8c047c2ef56049ac90d663ea63b103bc
出典データセット
uspto-grants-2002_02
特許番号
US06348624B1

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