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

HRID 1745827

反応式

HRID 1745827 の反応式
C(NC(C)C)(C)C.C([Li])CCC.[F:13][C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=1[Br:21].[Cl:22]C(Cl)(Cl)C(C(Cl)(Cl)Cl)=O>O1CCCC1>[Cl:22][C:19]1[C:14]([F:13])=[C:15]([Br:21])[CH:16]=[CH:17][C:18]=1[F:20]

参加物

6

反応物 4

HCID 7912DiisopropylamineHCID 8303HexachloroacetoneHCID 676741-Bromo-2,4-difluorobenzeneHCID 178418339Butyllithium

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of 19 ml (0.135 mole) of diisopropylamine in 125 ml of tetrahydrofuran (THF) 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-9b250c814545404cae096bdcd1837b3d
出典データセット
uspto-grants-2006_03
特許番号
US07019143B2

関連ノート

読み込み中…