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

HRID 1455487

반응식

HRID 1455487 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

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 to room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.

후처리

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

출처 및 근거

ORD 기록
ord-fe1a5e8222024fb9934e82e295db050f
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07482454B2

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